Category: iodides-buliding-blocks

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. HPLC of Formula: INa

Complex (-)-2 (0.29g, 0.32mmol) was dissolved in dichloromethane (50mL) and treated with excess concentrated hydrochloric acid (2mL) at room temperature for 5min. The mixture was then washed with water (3×50mL). Next, sodium iodide (0.1g) in water (50mL) was added and stirred vigorously for 3min. The organic layer was washed with water (3×50mL) and dried (MgSO4). The solvent was removed and the complex (-)-3 was isolated by column chromatography on a silica column with dichloromethane (0.19g, 70%). [alpha]D=-78.6 (c 0.14, CH2Cl2). Mp: 85-86C. Anal. Calcd for C26H26As2I2Pd: C, 36.8; H, 3.1. Found: C, 36.9; H, 3.2. 1H NMR (CDCl3, delta): 1.48 (s, 3H, =CCH3), 1.57 (s, 3H, =CCH3), 2.05 (dd, 3JHH=9.5, 2JHH=13.6Hz, 1H, CHCH2), 2.55 (d, 2JHH=13.0Hz, 1H, CHCH2), 2.96 (dt, 3JHH=2.1, 3JHH=9.4Hz, 1H, CHCH2), 3.07 (d, 3JHH=2.1Hz, 1H, AsCH), 3.52 (d, 3JHH=2.6Hz, 1H, AsCH), 7.37-8.02 (m, 15H, aromatics). 13C NMR (CDCl3, delta): 14.3, 15.7, 30.5, 31.4, 52.2, 56.3, 128.6, 129.1, 129.8, 129.9, 130.0, 130.9, 131.0, 131.1, 131.3, 131.6, 133.3, 133.7, 134.3, 135.8.

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

Reference:
Article; Yao, Weiwei; Ma, Mengtao; Wang, Weifan; Cheng, Jianming; Xu, Li; Pullarkat, Sumod A.; Leung, Pak-Hing; Tetrahedron Asymmetry; vol. 25; 15; (2014); p. 1100 – 1103;,
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1878-94-0, name is 2-(4-Iodophenoxy)acetic 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. Application In Synthesis of 2-(4-Iodophenoxy)acetic acid

Example 3; A. Podophyllotoxin-4-O-ester of 4-iodophenoxyacetic acid (000614); The mixture of podophyllotoxin (41 mg, 0.1 mmol), 4-iodophenoxyacetic acid (55 mg, 0.2 mmol), EDCI (40 mg, 0.14 mmol), DMAP (2 mg, 0.02 mmol) and dichloromethane (5 ml) were stirred in the room temperature for 20 h, then dichloromethane (20 ml) was added to the solution. Organic layer was washed with water (20 ml), saturated NaHCO3 aqueous solution (10 ml) and brine (20 ml), and then dried over MgSO4. After the solvent was removed under reduced pressure, the resulting liquid was separated by column chromatography (eluent: ethyl acetate and petroleum ether) to afford 35 mg podophyllotoxin-4-O-4-iodophenoxyacetate, mp. The chemical structure analysis was performed by 1HNMR (CDCl3, 600 MHz); delta 7.60 (t, 2H, Ar-H), 6.69 (d, 2H, Ar-H), 6.61 (s, 1H, Ar-H), 6.53 (s, 1H, Ar-H), 6.36 (s, 2H, Ar-H), 5.98 (d, 3H, OCH2O), 4.74 (q, 2H, COCH2O), 4.60 (d, 1H, H4), 4.34 (t, 1H, H11), 4.20 (t, 1H, H11), 3.81 (s, 3H, OCH3), 3.74 (s, 6H, OCH3), 2.91 (d, 1H, H2), 2.85 (m, 1H, H3).

The synthetic route of 1878-94-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yang, Li-Xi; US2005/4169; (2005); A1;,
Iodide – Wikipedia,
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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. 916792-62-6, name is 3-Fluoro-2-iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 916792-62-6

2-lodo-3- fluorobenzonitrile (2.5 g, 10.3 mmol) and 2-tributylstannane pyrimidine (3.7g, 10.0 mmol) were combined and dissolved in degassed DME (18 ml) then purged with bubbling N2 for 5 minutes. The reaction was treated withPd(PPh3)4 (577 mg, 0.5 mmol) and then purged with bubbling for 5 minutes in a sealed vessel and then heated in microwave at 160 oC for 90 min. The reaction was cooled and filtered through celite and concentrated to minimum volume and the ppt the formed was diluted with hexanes (40 ml) and cooled to 0 oC then filtered. The solid purified (FCC) (20-100% EA / hex) to give 3-fluoro- 2-(pyrimidin-2-yl)benzonitrile. 1 H NMR (400 MHz, CDCI3): 8.93 (d, J = 4.9 Hz, 2H), 8.14 (dd, J = 9.6, 2.7 Hz, 1 H), 7.86 (dd, J = 8.6, 5.3 Hz, 1 H), 7.36 (t, J = 4.9 Hz, 1 H), 7.32 – 7.24 (m, 1 H).

The synthetic route of 916792-62-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; CHAI, Wenying; LETAVIC, Michael, A.; LY, Kiev, S.; PIPPEL, Daniel, J.; RUDOLPH, Dale, A.; SAPPEY, Kathleen, C.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; SOYODE-JOHNSON, Akinola; STOCKING, Emily, M.; SWANSON, Devin, M.; WO2011/50198; (2011); A1;,
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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. 25309-64-2, name is 1-Ethyl-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-Ethyl-4-iodobenzene

General procedure: In a 25 mL reaction tube, Mn(OAc)3.2H2O(10 mol%), DABCO (2.5 equiv.) and a stirring bar were added. Then iodobenzene(1 mmol), phenyl acetylene (1 mmol) and PEG-400 were injected by syringe. The reaction tube was closed and transferred to a 70 C oil bath for 19-24 hours. After the reaction completed, cool down the reaction mixture to room temperature. Water (2 mL) was added and the reaction mixture was extracted with ethyl acetate and then concentrated and purified by column chromatography.

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

Reference:
Article; Qi, Xinxin; Jiang, Li-Bing; Wu, Xiao-Feng; Tetrahedron Letters; vol. 57; 15; (2016); p. 1706 – 1710;,
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Application of 25252-00-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 25252-00-0 as follows.

Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid (49.5 g) in CH2Cl2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiBH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.0 g (99% of theory)

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim Vetmedica GmbH; KLEY, Saskia; REICHE, Dania Birte; (42 pag.)EP3096765; (2018); B1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, molecular formula is C8H4F13I, 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. Computed Properties of C8H4F13I

General procedure: Perfluoroalkylethyl iodide (1.0 mol equiv.) (3-4 mmol) and NaN3 (1.2 mol equiv.) were added to dry DMSO (2 mL) in a 10 mL CEM microwave glass reactor tube, a magnetic stirring bead added and the system sealed. The tube was subjected to stirring and microwave irradiation at 250 W and 65 C for 1 h then immediately cooled to r.t.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2043-57-4, its application will become more common.

Reference:
Article; Francis, Dominic V.; Miles, D. Howard; Mohammed, Adnan I.; Read, Roger W.; Wang, Xiaobei; Journal of Fluorine Chemistry; vol. 132; 11; (2011); p. 898 – 906;,
Iodide – Wikipedia,
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Reference of 64248-58-4,Some common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, molecular formula is C6H3F2I, 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.

Intermediate 7: Ethyl 1-(3,4-difluorophenyl)-5-methyl-1H-1 ,2,3-triazole-4-carboxylate; To a mixture of 1 ,2-difluoro-4-iodobenzene (1 g, 4.17 mmol) and ethyl 2-butynoate (0.484 ml_, 4.17 mmol) in water (0.444 ml)/DMS0 (4 ml) at room temperature were added L-proline (0.096 g, 0.833 mmol), sodium carbonate (0.088 g, 0.833 mmol), sodium azide (0.325 g, 5.00 mmol), sodium l-ascorbate (0.083 g, 0.417 mmol) and copper(ll) sulfate pentahydrate (0.052 g, 0.208 mmol) (in this order) and the mixture was heated at 65 0C overnight. On cooling to room temperature, the mixture was quenched with aqueous ammonia (1 ml) and EtOAc (20ml) and water (20 ml) were added. The two phases were separated and the aqueous phase was extracted with EtOAc (3 x 30 ml). The organic phases were combined and washed with water/brine (50ml) repeatedly. The organic phases were dried over sodium sulfate, filtered and the solvent was evaporated to afford a crude product that was purified by MDAP to afford the title compound (23.9%); MH+=267.9; 1HNMR (DMSO, 400 MHz): 1.34 (3H t), 4.36 (2H, q), 7.57 (1 H m), 7.76 (1 H m), 7.94 (1 H m).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2-Difluoro-4-iodobenzene, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/115486; (2009); A1;,
Iodide – Wikipedia,
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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. 3058-39-7, name is 4-Iodobenzonitrile, A new synthetic method of this compound is introduced below., Formula: C7H4IN

The compound 4-cyanoiodobenzene 1a (1.0 mmol), DMSO (5 ml), Cs2CO3 (2.0 mmol), and phenol 2a (1.2 mmol) were added to the mixture, and the mixture was stirred at room temperature for 10 minutes. Then placed in an 80 C oil bath, reacted under lightAfter 10 h, after TLC detection reaction, the reaction solution was filtered, extracted and subjected to column chromatography to obtain the target product 4a, yield 79%.

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; China Three Gorges University; Wang Long; Liu Na; Yang Qingqing; Hu Weimin; (8 pag.)CN109824544; (2019); A;,
Iodide – Wikipedia,
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These common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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. category: iodides-buliding-blocks

Add triethylamine (6. 2 mL, 44 mmol), copper (I) iodide (120. 3 mg, 1. 10 mmol) and bis (triphenylphosphine) palladium (II) dichloride (386 mg, 0. 55 mmol) to a solution of 3-bromo-5-ethynylpyridine, (prepared essentially as described in PREPARATION 23), (2. 0 g, 11 mmol) and 1-iodo-3-trifluoromethylbenzene (1. 53 mL, 11 mmol) in ethyl acetate (12 mL). Stir at room temperature for 18 h. Concentrate and purify the residue by silica gel chromatography, eluting with 100 : 0 to 100 : 50 hexanes : ethyl acetate to give the title compound (2. 1 g, 61%). 1H NMR (300 MHz, CDCl3) 6 7. 52 (t, J = 8. 0 Hz, 1H), 7. 64 (d, J = 8. 0 Hz, 1H), 7. 71 (d, J = 8. 0 Hz, 1H), 7. 80 (br s, 1H), 7. 98 (t, J = 2. 2 Hz, 1H), 8. 64 (d, J = 2. 2 Hz, 1H), 8. 68 (d, J = 2. 2 Hz, 1H) ; MS (ES) : m/z = 326 [M+H] +.

The synthetic route of 1-Iodo-3-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/94822; (2005); A1;,
Iodide – Wikipedia,
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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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., Formula: C7H4ClIO2

[0256] A I L 4-necked flask equipped with thermometer and mechanical stirrer (operating at 150 RPM) was charged with 2-chloro-5-iodobenzoic acid (14.1 g, 0.05 mol), DCM (70.5 mL) and oxalyl chloride (5.5 mL, 0.06 mol). After stirring for 10 min, the mixture was cooled to 10 to 15 C and DMF (0.15 mL, 1.92 mmol) was added by syringe over 10 min in two boluses of 0.1 and 0.05 mL while keeping the reaction temperature below 20 C. After the addition was completed, the mixture was warmed to 25 C and stirred for 16 h. The mixture was concentrated and the residue was dried under vacuum at 30 C for 5 h to give 15.0 g of product as a white solid. Yield: 100%. LC-MS Method EGT-M-0013: 99 % Purity, 1H NMR (CDCI3, 400 MHz): 8.33 (d, J=2.4 Hz, 1H), 7.81-7.84 (dd, J=2.4 Hz, 8.4 Hz, 1H), 7.23 (d, J=8.4 Hz, 1H).

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERACOS, INC.; XU, Baihua; LV, Binhua; XU, Ge; SEED, Brian; ROBERGE, Jacques; WO2013/152476; (2013); A1;,
Iodide – Wikipedia,
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