Tag: M.W=200-300

Application of 852569-38-1, These common heterocyclic compound, 852569-38-1, name is 5-Chloro-4-fluoro-2-iodoaniline, 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.

Step 6.3. N-(5-chloro-4-fluoro-2-iodophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxamide Potassium t-butoxide (12.52 g, 111.6 mmol) is added at room temperature to a solution of 5-chloro-4-fluoro-2-iodoaniline (5.0 g, 22.3 mmol) in 250 mL of anhydrous THF under nitrogen. After stirring for 15 minutes, a solution of 1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxylic acid fluoride (5.67 g, 24.6 mmol) in 30 mL of anhydrous THF is added dropwise. The reaction mixture is stirred for 4 hours at room temperature and then poured into saturated aqueous NaHCO3 solution and extracted with EtOAc. The organic phase is washed with saturated aqueous NaCl solution, dried over Na2SO4 and concentrated to dryness. After purification by flash chromatography on silica (cyclohexene/EtOAc: 95/5 to 80/20), a red solid is obtained, which is purified by flash chromatography on amine phase (DCM) to give 2.84 g of a white solid (yield: 31%). LCMS (Method E): MH+= 404.0, RT = 2.29 min

Statistics shows that 5-Chloro-4-fluoro-2-iodoaniline is playing an increasingly important role. we look forward to future research findings about 852569-38-1.

Reference:
Patent; SANOFI; Benazet, Alexandre; Duclos, Olivier; Guillo, Nathalie; Lassalle, Gilbert; Macary, Karim; Viv, Valerie; EP2573073; (2013); 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. 612-55-5, name is 2-Iodonaphthalene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodonaphthalene

Bis(t?phenylphosphine)palladium (II) chloride (0 18 g, 0 26 mmol, 0 18 mol %) was added to a stirred solution of propargyl alcohol (8 43 mL, 144 8 mmol, 1 eq ), 2-iodonapthalene (36 g, 142 mmol), t?ethylamine (39 6 mL, 284 mmol, 2 eq ) and copper iodide (0 09 g, 0 49 mmol, 0 3 mol %) in tetrahydrofuran (750 ml) The mixture was stirred at 35 0C for 12 h under nitrogen atmosphere The mixture was then filtered through a bed of cehte and the filtrate was washed with ethyl acetate (200 ml) The filtrate was then concentrated in vacuo Purification by silica gel chromatography using 1 6 ethyl acetate/petrol as the eluting solvent afforded the desired compound (2 85 g, 1 1%) as a white solid 1H NMR (400 MHz, CDCl3) delta ppm 4 54 (2H, s, CH2), 7 45-7 49 (3eta, m, ArH), 7 75-7 81 (3eta, m, ArH), 7 95 (1eta, s, ArH)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 612-55-5.

Reference:
Patent; DOV PHARMACEUTICAL, INC.; WO2008/57575; (2008); A2;,
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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H4FIO2

General procedure: 1-acetoxyethanephosphonate-5-fluoro -1, 2- […] -3-(1H)-one (AFBX (2)) of synthetic The flask 2-iodo-5-fluorobenzoate 1330 mg (5mmol), then adding acetic acid 40 ml agitated until uniform. 3-hydroxybenzoic acid (purity 65%)overload Chloropyridin 1590 mg (6mmol) at a time and then adding a 24 60 C. The reaction liquid is cooled to 0 C, ether is added. The precipitate is filtered by deposition, vacuum drying in 1-acetoxyethanephosphonate-5-fluoro -1, 2- […] -3-(1H)-one (AFBX (2)) 770 mg (yield 48%)is obtained.

According to the analysis of related databases, 52548-63-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tokyo Chemical Industry Co., Ltd.; Togo, Hideo; Inuma, Masataka; Moriyama, Katsuhiko; Takatsuki, Kenichi; (9 pag.)JP2015/63501; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 14452-30-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 14452-30-3, name is 1-(3-Iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a 10 mL glass screw cap tube capped with a rubber septum, palladium acetate Pd(OAc)2, (5 mg, 0.023 mmol), 1,3-bis(diphenylphosphino)propane dppp, (9 mg, 0.023 mmol) were introduced under argon atmosphere. Then, 3 mL of freshly distilled toluene) were added under argon. The mixture was stirred for 10 min to allow formation of the catalyst. Then securinine 1 (100 mg, 0.46 mmol), potassium carbonate (K2CO3, 127 mg, 0.92 mmol) and the desired iodoarene (0.92 mmol) were added. The septum was replaced by a screw cap, and the mixture was stirred at 130 C, in an oil bath. After 24 h stirring, the reaction mixture was brought to room temperature and diluted with ethyl acetate (5 mL). The reaction mixture was filtered through a pad of Celite eluting with AcOEt (20 mL). The organic layer was extracted with a saturated aqueous solution of sodium hydrogen carbonate (10 mL) and brine (10 mL). The organic layer was then dried over anhydrous magnesium sulfate, filtered and concentrated to dryness. Purification by flash column chromatography on silica gel (pentane-ethyl acetate) affords the desired coupling product. 4.1.2.1.16 (6S,11aR,11bS)-5-(3-Acetylphenyl)-9,10,11,11a-tetrahydro-8H-6,11b-methanofuro[2,3-c]pyrido[1,2-a]azepin-2(6H)-one (2p) Yield: 60%. Orange oil; Rf 0.42 (petroleum ether-AcOEt, 50:50); [alpha]D20 – 475 (c = 0.10, CHCl3); 1H NMR (300 MHz, CDCl3): delta = 8.09 (s, 1H), 7.92 (d, J = 7.8 Hz, 1H), 7.69 (d, J = 7.8 Hz, 1H), 7.50 (dd, J = 7.8 Hz, 1H), 6.86 (d, J = 1.3 Hz, 1H), 5.59 (s, 1H), 4.36 (d, J = 4.3 Hz, 1H), 2.91-2.85 (m, 1H), 2.65-2.60 (m, 4H), 2.32-2.17 (m, 2H), 1.90-1.80 (m, 2H), 1.67-1.45 (m, 4H), 1.25-1.13 (m, 1H); 13C NMR (75 MHz, CDCl3): delta = 197.3, 173.6, 169.9, 149.2, 138.9, 137.5, 130.5, 129.2, 125.8, 116.3, 105.1, 89.0, 62.9, 61.6, 48.7, 41.8, 27.3, 26.5, 25.7, 24.0. MS (CI, NH3): m/z = 336 [M+ + H]; HRMS calcd for C21H21NO3H [M+ + H]: 336.15942; found: 336.15882, error = 1.8 ppm.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-(3-Iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Perez, Marc; Ayad, Tahar; Maillos, Philippe; Poughon, Valerie; Fahy, Jacques; Ratovelomanana-Vidal, Virginie; European Journal of Medicinal Chemistry; vol. 109; (2016); p. 287 – 293;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 31599-61-8, These common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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.

General procedure: A mixture containing aryl halide (5.0 mmol), styrene(5.0 mmol), the palladium complex 5a (0.005 mmol) and potassium carbonate (1.06 g, 10.0 mmol) in methanol (20 ml) was refluxed for 2 h, as mentioned in Table 4. After the reaction, the solvent was evaporated, the product was poured into water, extracted with diethyl ether, dried over Na2SO4 and passed through a 1200 silica column (60-120 mesh). Upon evaporation of the ether, solid pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation and the products characterized by 1H NMR spectra (Table 7).

Statistics shows that 4-Iodo-1,2-dimethylbenzene is playing an increasingly important role. we look forward to future research findings about 31599-61-8.

Reference:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Brandao, Paula; Felix, Vitor; Chattopadhyay, Surajit; Polyhedron; vol. 79; (2014); p. 43 – 51;,
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. 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H9IO2

General procedure: A mixture of aryl halide (1 mmol), phenylboronic acid(1.2 mmol), K2CO3 (2 mmol), Fe3O4-AuSF-SBA-15 nanocatalyst(50 mg or 0.64 mmol% of Au) and 5 mL of C2H5OH/H2O (1:1) wereadded to a 25 mL round-bottom flask and stirred at 80 C forappropriate times. After completion the reaction (controlled byTLC), the mixture was cooled and the catalyst was recovered by amagnet and washed three times with ethyl acetate and ethanol.The combined organic layer was dried over MgSO4. Then the solventwas evaporated and the residue was purified by column chromatographyand characterized by its 1H NMR, 13C NMR andmelting point.

The synthetic route of 5460-32-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Khodaei, Mohammad Mehdi; Dehghan, Mahsa; Polyhedron; vol. 162; (2019); p. 219 – 231;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 3930-83-4,Some common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, molecular formula is C7H6INO, 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: To a 10 mL reaction tube were added MCM-41-L-Proline-CuBr(135 mg, 0.1 mmol), 2-halobenzamide 1 (1.0 mmol), benzylamine derivative 2 (2.0 mmol), K2CO3 (3.0 mmol), and DMSO (3 mL). The reaction mixture was stirred at 110 or 120 C under air for 6-12 h.After being cooled to room temperature, the reaction mixture was diluted with 20 mL of EtOAc, and filtered. The MCM-41-L-Proline-CuBr complex was washed with distilled water (2 5 mL) and ethanol (2 5 mL), and reused in the next run. The filtrate was washed with water (2 10 mL) and dried over MgSO4. After being concentrated in vacuo, the residue was purified by flash column chromatography on silica gel (petroleum ether/EtOAc 3:1 to 2:1)to afford the target product 3.

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yan, Nan; You, Chongren; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 897; (2019); p. 161 – 169;,
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. 23399-70-4, name is 5-Chloro-2-iodotoluene, A new synthetic method of this compound is introduced below., Computed Properties of C7H6ClI

Specific operation: In a 25 mL reaction flask equipped with a magnetic stirrer, a metal catalyst palladium acetate (6.7 mg, 0.03 mmol), triphenylphosphine (20.0 mg, 0.075 mmol) was added,S-2-bromophenyl-S-methyliminosulfanone (70.0 mg, 0.3 mmol), norbornene (56.4 mg, 0.6 mmol), potassium carbonate (82.8 mg, 0.6 mmol),Protect with nitrogen (at least three nitrogen cycles), add acetonitrile (3 ml) and 5-chloro-2-iodotoluene (90.9 mg, 0.36 mmol) successively in a nitrogen stream and close the vessel.The reaction solution was heated to 80 C. for about 12 h, and the reaction was complete by TLC.After the treatment, the reaction solution was first diluted with 15 ml of ethyl acetate, and then the inorganic substances such as the catalyst and the alkali were removed by suction filtration through a sand funnel containing silica gel.The resulting filtrate was separated by flash column chromatography to give the pure product 9-chloro-5,7-dimethyldibenzo[c,e][1,2]thiazine-5-oxide compound 3l. Yield: 69%.

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; Jiangxi Normal University; Chen Zhiyuan; Zhou Hao; Wang Xiumei; (17 pag.)CN107987034; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 58313-23-8, These common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, 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.

General procedure: A dry and argon-flushed Schlenk-flask, equipped with a magnetic stirring bar and a rubberseptum, was charged with FeCl2 (10 mol%, 99.5% pure), the corresponding electrophile (1.0equiv) and freshly distilled THF. Thereupon, the benzylic manganese(II) chloride solution (1.05-1.10 euqiv) was dropwise added at 0 C. After the addition was complete, the reaction mixturewas stirred for a given time at the prior adjusted temperature and then allowed to warm toroom temperature. The reaction completion was monitored by GC-analysis of quenched aliquots.A saturated aqueous solution of NH4Cl was added and the aqueous layer was extracted threetimes with Et2O or EtOAc (3 × 50 mL). The combined organic layers were dried over MgSO4,filtered and concentrated under reduced pressure. Purification of the crude products by flashcolumn chromatography afforded the desired products.

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Benischke, Andreas D.; Breuillac, Antoine J. A.; Moyeux, Alban; Cahiez, Gerard; Knochel, Paul; Synlett; vol. 27; 3; (2016); p. 471 – 476;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 58313-23-8,Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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 83; (IS, 2R) and (1R, 2S)-3-(2-(4-chlorophenyl)-2′-oxospiro[cyclopropane-l,3′-indoline]- l’-yl)benzoic acid; Synthesis of (IS, 2R) and (1R, 2S)-methyl-3-(2-(4-chlorophoxospiro[cyclopropane-l,3′-indoline]-l’-yl)benzoateA Schlenk tube was charged with Cul (9.6 mg, 0.05 mmol, 5.0 mol %), racemic (1R, 2S) and (I S, 2R)-2-(4-chlorophenyl)spiro[cyclopropane-l,3′-indolin]-2′-one (270 mg, 1.0 mmol), and K2C03 (276 mg, 2.0 mmol), evacuated, and backfilled with argon. N, iV- Dimethylethylenediamine (1 1 /L, 0.10 mmol, 10 mol %), ethyl 3-iodobenzoate (278.8 mg, 1.01 mmol), and acetonitrile (1.5 mL) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 80 C for 23 hours. HPLC monitored the reaction finished. The solvent was removed under reduced pressure. The residue was purified by flash column chromatography column (gradient elution, 5-10 % ethyl acetate in petroleum ether) to give the title compound as a yellow powder (290 mg, 72 %). LC/MS m/e calcd. for C24Hi8ClN03: 403, observed (M+H)+: 404.1.

The synthetic route of 58313-23-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; CHEN, Li; HUANG, Mengwei; FENG, Lichun; HE, Yun; YUN, Hongying; WO2011/69298; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com