Month: April 2021

Application of 31827-94-8,Some common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 869500-07-2, name is 1-Bromo-2-iodo-3-methylbenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 869500-07-2, name: 1-Bromo-2-iodo-3-methylbenzene

A mixture of 1-bromo-2-iodo-3-methylbenzene (0.46g), {3-[(ethyloxy)- carbonyl] phenyl}boronic acid (0.20g), tetrakis(triphenylphosphine)palladium(0) (60mg), potassium carbonate (0.71g), toluene (6ml) and ethanol (6ml) was stirred under reflux under nitrogen for 3h. The mixture was partitioned between water (40ml) and ether (40ml) and the aqueous layer extracted with ether (15ml). The combined ether extracts were dried (MgS04), evaporated and the residue purified by flash chromatography eluting with 2% ethyl acetate in isohexane to afford the title compound (0.22g). LC/MS Rt = 4.1 min, [MH+] 319/321.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2005/108369; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 401-81-0

6b (458 mg, 2.00 mmol) in 1.0 ml of dry THF was initially introduced into a dry 10 ml microwave tube filled with argon and with a magnetic stirrer core and septum, and Zn(TMP)2.2LiCl.2MgCl2 in THF (3.2 ml, 0.37 M, 0.60 equivalent) was added at 25 C. The microwave tube was closed and the reaction was started. After 2 h in the microwave oven (120 W, 80 C.) the metallization was complete (GC analysis of reaction samples to which a solution of I2 in THF had been added indicated a conversion of more than 98%). After the reaction mixture had been cooled to room temperature, this was added to a solution of 3-CF3-C6H4-I (680 mg, 1.2 equivalents), Pd(dba)2 (5 mol %) and Tfp (10 mol %) in dry THF (2.5 ml). After stirring at 25 C. for 15 h, the reaction was ended by addition of saturated NH4Cl solution (30 ml). The aqueous phase was extracted with ethyl acetate (5¡Á30 ml), dried over MgSO4 and concentrated under reduced pressure. The crude product was purified by filter column chromatography (silica gel; Et2O/pentane 1:15); 7b (680 mg, 76%) was obtained as a yellow oil.

According to the analysis of related databases, 401-81-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ludwig Maximilians Universitat Munchen; US2010/160632; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H4F3I

Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. The t-butyl ester pyran from Part A (1.0 g, 2.04 mmol) and [1,1?-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with CH2Cl2 (1:1) (0.083 g, 0.102 mmol, Aldrich) were added, and the resulting dark mixture was stirred overnight at 69 C. under N2. Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. This mixture was added to the original flask, and the resulting mixture was stirred overnight at 70 C. under N2. An additional portion of the Pd catalyst (same amount used above) was added to the mixture, and the resulting mixture was stirred at 70 C. overnight under N2. Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. This mixture was added to the original flask along with another portion of the Pd catalyst (same amount used above), and the resulting mixture was stirred overnight at 70 C. under N2. The mixture was allowed to cool to ambient temperature, and 50 mL each of saturated NH4Cl(aq) and deionized water were added to the mixture. The mixture was then stirred for 15 min. Afterward, the mixture was further diluted with 200 mL of ethyl acetate and filtered through a pad of Celite . The filter cake was washed with 50 mL each of deionized water and ethyl acetate. The layers were separated, and the organic layer was washed with 100 mL of saturated NaCl(aq), dried over MgSO4, and concentrated in vacuo to form a brown oil (1.43 g). Chromatography (silica, ethyl acetate/hexanes) afforded 0.80 g (78% yield) of a yellow oil.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Barta, Thomas E.; Becker, Daniel P.; Bedell, Louis J.; Boehm, Terri L.; Brown, David L.; Carroll, Jeffery N.; Chen, Yiyuan; Fobian, Yvette M.; Freskos, John N.; Gasiecki, Alan F.; Grapperhaus, Margaret L.; Heintz, Robert M.; Hockerman, Susan L.; Kassab, Darren J.; Khanna, Ish K.; Kolodziej, Stephen A.; Massa, Mark A.; McDonald, Joseph J.; Mischke, Brent V.; Mischke, Deborah A.; Mullins, Patrick B.; Nagy, Mark A.; Norton, Monica B.; Rico, Joseph G.; Schmidt, Michelle A.; Stehle, Nathan W.; Talley, John J.; Vernier, William F.; Villamil, Clara I.; Wang, Lijuan J.; Wynn, Thomas A.; US2005/9838; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, molecular formula is C8H9I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 2-Iodo-1,3-dimethylbenzene

General procedure: To a reaction tube containing (17alpha-20E)-21-(tri-n-butylstannyl)-19-norpregna-1,3,5(10)20-tetraene-3,17beta-diol, 2a, were added a few crystals of 2,6 di-tert-butyl-4-methylphenol and the substituted phenyl/xylyl iodide. The tube was dried under vacuum for 24 h, then exchanged with argon at least four times. Tetrakis(triphenylphosphine) palladium (0) (0.024 g, 0.02 mmol) and dried, degassed toluene (5 mL) were added and the reaction was heated at 110 C for 6-18 h. After cooling to room temperature, the reactuib mixture was transferred to a flask with ethyl acetate (50 mL), activated charcoal was added, the mixture heated to boiling, and then filtered through a Celite pad. To the filtrate containing the substituted phenyl vinyl estradiol derivative, fluorsil (4-8 g) was added and then mixture was evaporated to dryness. Hexane was then added to the slurry and the mixture was again evaporated to dryness. The substituted phenyl vinyl estradiol was isolated using flash chromatography and characterized by 1H and 13C NMR, elemental analysis

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 608-28-6, its application will become more common.

Reference:
Article; Hanson, Robert N.; McCaskill, Emmett; Tongcharoensirikul, Pakamas; Dilis, Robert; Labaree, David; Hochberg, Richard B.; Steroids; vol. 77; 5; (2012); p. 471 – 476;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a 500-mL round-bottom flask reactor, methyl 5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis(triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) were stirred together with toluene (125 mL), tetrahydrofuran (125 mL), and water (50 mL) for 10 hrs at 80 C. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford . (75.0 g, 60.1%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; Cha, Soon-Wook; Park, Young-Hwan; Yoon, Seo-Yeon; Shim, So Young; (152 pag.)US2017/18723; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 25309-64-2,Some common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, molecular formula is C8H9I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 1Preparation of pinacol ester of 4-ethylphenylboronic acid In a 2 necks Schlenk type flask, provided with a magnetic stirring bar and topped by a coolant, 4-ethylbenzene iodide (0.232 g, 1 mmol), pinacolborane (0.128 g, 1 mmol) and triethylamine (59 mg, 1 mmol) are added to 10 ml of a distilled THF solution containing magnesium turnings (24 mg, 1 mmol). The reactive mixture is stirred for approximately 15 hours at THF reflux.At the end of the reaction, the crude reaction product is hydrolyzed by 20 ml of neutral water and extracted by diethyl ether (3¡Á40 ml). The joined organic phases are washed by 2¡Á50 ml of neutral water then dried on MgSO4. After solvent evaporation, the obtained yield is of 96% with a total conversion of the starting iodide (yield/conversion of 96%). The resulting boronic ester is analyzed by GC, NMR 1H and 13C and GC/MS.Characterizations:NMR 1H, 7.74 (2H, D, 3 Hz); 7.22 (2H, D, 3 Hz); 2.66 (2H, Q, 3 Hz); 1.34 (12H, s); 1.24 (3H, T, 3 Hz).NMR 13C, 146.68; 133.87; 127.23; 126.31; 82.58; 28.08; 23.82; 14.42.Mass spectrometry: 232-231 (M+, 6-2%); 217-216 (8-2%); 147 (19%); 146-145 (71-15%); 134 (17%); 133 (100%); 132-131 (63-21%); 118 (18%); 117 (51%); 116-115 (17-4%); 105 (18%); 104 (10%); 91 (11%); 85 (14%); 77-76 (9-2%).Ultimate Analyses:calculated %: C: 72.44%; H: 9.12%; B: 4.66%.obtained %: C: 70.22%; H: 9.25%; b: 4.39%.

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Universite De Nice Sophia Antipolis; US2011/282090; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 452-79-9,Some common heterocyclic compound, 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene, molecular formula is C7H6FI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of 3-fluoro-4-iodotoluene (2.26 g, 9.58 mmol), N-bromosuccinimide (2.03 g, 11.49 mmol) and benzoyl peroxide (5 mol %, 116 mg, 0.48 mmol) in carbon tetrachloride (5 ml) was stirred at reflux for 20 hours, cooled, diluted with dichloromethane and filtered. The purple coloured filtrate was washed with saturated sodium thiosulphate solution (aq) (20 ml). The organic layer was separated, dried over sodium sulphate and the solvent removed by rotary evaporation to give the title compound as a yellow oil (2.58 g, 86%).1H-NMR (250 MHz, CDCl3): delta 7.72 (1H, m), 7.11 (1H, m), 6.94 (1H, m), 4.41 (2H, s).

The synthetic route of 452-79-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; US2010/137276; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 52548-63-7

To a solution of 1H-pyrrolo[2,3-c]pyridine (70 g, 0.59 mol) in MeOH (1,050 mL) and H2O (350 mL) was added KOH (83 g, 1.48 mol) and tert-butyl 3-oxopiperidine-1- carboxylate (259 g, 1.30 mol). The resulting mixture was stirred at 75-80 oC (oil bath temperature) for 18 h. The reaction mixture was concentrated under reduced pressure to remove MeOH, then H2O (700 mL) was added and the mixture was extracted with EtOAc (3 ¡Á 1000 mL). The organic layers were filtered and the filtered cake was washed with EtOAc (2 ¡Á 150 mL) to afford tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4- dihydropyridine-1(2H)-carboxylate (75 g, 42% yield) as white solid. The organic layer was concentrated under reduced pressure to about 250 mL. The residue was stirred at 5-9 oC for 18 h. The residue was filtered and the filtered cake was washed with EtOAc (2 ¡Á 60 mL) to give a mixture of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6- dihydropyridine-1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4- dihydropyridine-1(2H)-carboxylate (1:3.5 via LCMS; (28 g, 16% yield) as white solid. tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine-1(2H)- carboxylate: Yield: 75 g (42%); Rt value: 0.570 (LCMS Method C); (M+H)+ = 300.1; 1H NMR (MeOD, 400 MHz): delta ppm 8.65-8.70 (d, J = 2.8 Hz, 1H), 8.05-8.15 (d, J = 5.6 Hz, 1H), 7.70-7.90 (m, 1H), 7.54 (s, 1H), 7.35-7.50 (m, 1H), 3.60-3.75 (m, 2H), 2.50-2.60 (t, J = 5.6 Hz, 2H), 2.00-2.10 (m,2H), 1.55-1.60 (m, 9H). Mixture of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6-dihydropyridine- 1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine- 1(2H)-carboxylate: Rt value: 0.568 (LCMS Method C); (M+H)+ = 300.1. A suspension of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine- 1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6-dihydropyridine- 1(2H)-carboxylate (1 g, 3.34 mmol, ~10:1 ratio of isomers), 5-fluoro-2-iodobenzoic acid (977 mg, 3.67 mmol), K2CO3 (1.15 g, 8.33 mmol), CuI (63 mg, 0.334 mmol) and 1,10- phenanthroline (60 mg, 0.334 mmol) in DMF (13 mL, 0.26 M reaction concentration) was degassed with N2 for 15 min. The reaction mixture was then placed under N2 and heated to 70 oC for 24 h. The reaction was then cooled to room temperature and filtered through a plug of Celite using a small amount of DMF to rinse the filter cake. The DMF solution was cooled to 0 oC and a 1N aq. HCl solution (~10 mL) was added, maintaining a pH of ~5, followed by the addition of H2O (~10 mL) and EtOAc for the extraction. The EtOAc layer was separated and the aqueous layer (pH~5) was extracted three additional times with EtOAc. The EtOAc layers were combined and washed with H2O followed by brine. After drying over Na2SO4, the EtOAc layer was evaporated and the resulting residue was dried under high vacuum overnight to afford ~2 grams of crude 2-(3-(1-(tert-butoxycarbonyl)-1,4,5,6-tetrahydropyridin-3-yl)-1H-pyrrolo[2,3-c]pyridin- 1-yl)-5-fluorobenzoic acid and 2-(3-(1-(tert-butoxycarbonyl)-1,2,5,6-tetrahydropyridin-3- yl)-1H-pyrrolo[2,3-c]pyridin-1-yl)-5-fluorobenzoic acid (>10:1 ratio of isomers). The crude material was used directly for the next step without further purification. LCMS: 5.748 min (LCMS Method G): 438.47 (M + 1).1H NMR (400 MHz, CDCl3): delta 8.52-8.48 (m, 1H), 8.20-8.15 (m, 1H), 8.07 (bs, 1H), 8.01 (s, 1H), 7.85 (d, 1H, J = 8.4 Hz), 7.76 (s, 1H), 7.55 (bs, 1H), 7.42 (d, 1H, J = 5.2 Hz), 3.67 (bs, 2H), 2.50-2.47 (m, 2H), 2.06-2.01 (m, 2H), 1.54 (s, 9H). To a solution of the crude mixture from Step 2, (3.34 mmol), N-methylpropan-2- amine (731 mg, 10.02 mmol) and iPr2NEt (1.74 mL, 10.02 mmol) in EtOAc (9 mL) was added a 50 wt% solution of T3P in EtOAc (6 mL, 10.02 mmol) dropwise at ~10 oC. The reaction was stirred for 2 h, cooled to 0 oC, and a 1N aq. NaOH solution (~10 mL) was slowly added. The EtOAc layer was separated and the aqueous layer was extracted twice with EtOAc. The EtOAc layers were combined and washed with sat. NH4Cl, H2O, and then brine. After drying over Na2SO4, the EtOAc layer was evaporated to afford 1.65 grams of crude tert-butyl 5-(1-(4-fluoro-2-(isopropyl(methyl)carbamoyl)phenyl)-1H- pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine-1(2H)-carboxylate (purity: ~90% based on LCMS analysis). This material was used directly for the next step without further purification. LCMS: 6.247 min (LCMS Method G); 493.55 (M+1).1H NMR (400 MHz, CDCl3) The title compound was observed as a mixture of rotamers by NMR, the major rotamer isomer peaks were tabulated and are provided: delta 8.07-8.68 (m, 1H), 8.35-8.32 (m, 1H), 7.88 (d, 1H, J = 5.2 Hz), 7.62 (bs, 1H), 7.55-7.52 (m, 1H), 7.43-7.41 (m, 1H), 7.29-7.18 (m, 2H), 4.65-4.75 (m, 1H), 3.60-3.65 (m, 2H), 2.69 (s, 3H), 2.40-2.45 (m, 2H), 1.90-2.00 (m, 2H), 1.57 (s, 9H), 0.95-0.94 (m, 3H), 0.56-0.59 (m, 3H).

The synthetic route of 52548-63-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VITAE PHARMACEUTICALS, INC.; CACATIAN, Salvacion; CLAREMON, David A.; DONG, Chengguo; FAN, Yi; JIA, Lanqi; LOTESTA, Stephen D.; SINGH, Suresh B.; VENKATRAMAN, Shankar; YUAN, Jing; ZHENG, Yajun; ZHUANG, Linghang; (285 pag.)WO2018/53267; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

7681-82-5, name is Sodium iodide, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 7681-82-5

General procedure: A typical example is exemplified by the synthesis of 4b: To a stirred solution of TMEDA (1.36 mL,9 mmol) in hexane (5 mL) was added dropwise at ice bath temperature n-butyllithium (9 mmol) in hexane followed by acetophenone trimethylsilyl enol ether 1 (576 mg, 3 mmol), and the mixture was stirred for 24 h at room temperature. In a separate flask, a mixture of bismuth(III) chloride (315.5 mg,1 mmol) and tris(4-methylphenyl)bismuthane (964 mg, 2 mmol) was stirred in ether (10 mL) at room temperature for 1 h. To the suspension of chlorobis(4-methylphenyl)bismuthane (ca. 3 mmol) thus formed was added sodium iodide (450 mg, 3 mmol) and a few drops of 15-crown-5 ether and the resulting yellowish mixture was stirred for 3 h at room temperature. To a suspension of the lithium compound previously prepared was added at room temperature magnesium dibromide diethyl etherate (775 mg, 3 mmol) followed by, at -30 C, a suspension of iodobis(4-methylphenyl)bismuthane(ca. 9 mmol), and the resulting mixture was stirred for 1 h, during which time the temperature was raised to ambient temperature. The reaction mixture was poured into brine (50 mL) and extracted with ethyl acetate (50 mL ¡Á 3). The combined extracts were concentrated to leave an oily residue, which was purified by chromatography (silica gel) using hexane-ethyl acetate (5:1) as the eluent to afford 4b in 30% yield (459 mg, 0.9 mmol). Because 4a, 4f and 10 underwent decomposition when purified by chromatography on silica gel, these compounds were converted into the corresponding halobismuthanes 5a, 5f and 11, respectively, without isolation.

The synthetic route of 7681-82-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Murafuji, Toshihiro; Tomura, Mai; Ishiguro, Katsuya; Miyakawa, Isamu; Molecules; vol. 19; 8; (2014); p. 11077 – 11095;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com