Author: Jessica.F

Related Products of 33348-34-4, 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. 33348-34-4, name is 4-Amino-3-iodobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: In a flame-dried flask, AlMe3 (2 M in toluene, 1.11 mL, 2.18mmol, 1.2 equiv) was added to dry toluene (3.0 mL) under anitrogen atmosphere. The mixture was cooled to 0 C, and the2-iodoaniline (2.0 mmol, 1.1 equiv) in dry toluene (4.0 mL) was added. The mixture was stirred for a further 5 min at 0 C. Theice bath was removed, and the mixture was stirred for 20 min atroom temperature. The mixture was cooled to 0 C again, and cyclopentene carboxylate 2b (1.82 mmol, 1.0 equiv) in drytoluene (3.0 mL) was added dropwise over 2 min to the mixture. After stirring for 10 min at 0 C, the mixture was heated to 60 C, and stirring was continued for 16 h. After cooling to room temperature, HCl (1 M, 8.0 mL) was added. (Caution: gas evolution,exotherm.) The mixture was stirred for 15 min, then water (20 mL) and EtOAc (30 mL) were added. The mixture was extracted, the organic phase was separated, and the aqueous phase was re-extracted one more time with EtOAc (30 mL). Thecombined organic phases were washed with brine and dried (MgSO4). After filtration, the solvent was removed under reduced pressure, and the crude mixture was purified by column chromatography.

The chemical industry reduces the impact on the environment during synthesis 4-Amino-3-iodobenzonitrile. I believe this compound will play a more active role in future production and life.

Reference:
Article; Adeyemi, Ahmed; Wetzel, Alexander; Bergman, Joakim; Branalt, Jonas; Larhed, Mats; Synlett; vol. 30; 1; (2019); p. 82 – 88;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, 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. COA of Formula: C10H4F17I

The catalyst was separated from the reaction liquid obtained in Example 5 by filtration, and the unreacted olefin was removed with an evaporator, giving 47.5 g of solid CF3(CF2)7CH2CH2I. A 200-ml SUS autoclave was charged with 47.5 g (0.082 mol) of the obtained solid CF3(CF2)7CH2CH2I, 9.9g (0.090 mol) of potassium acrylate, 25 g of t-butanol (solvent), 0.6 g of hydroquinone (polymerization inhibitor) and 0.01 g of hydroquinone monomethyl ether (polymerization inhibitor), and a reaction was then carried out with stirring at 180C for 6 hours.. As a result, CF3(CF2)7CH2CH2OCOCH=CH2 was obtained at a CF3(CF2)7CH2CH2I conversion rate of 99% and at a selectivity of 88%.. The results of NMR analysis revealed that polymerization of CF3(CF2)7CH2CH2OCOCH=CH2 was not detected.

The synthetic route of 1-Iodo-1H,1H,2H,2H-perfluorodecane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daikin Industries, Ltd.; EP1457477; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 689291-89-2, A common heterocyclic compound, 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde, molecular formula is C7H4BrIO, 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.

Compound 12 (32.0 mg, 0.103 mmol), 46 (55.6 mg, 0.103 mmol), PdCl2(PPh3)2 (3.6 mg, 0.0051 mmol), and CuI (1.96 mg, 0.0103 mmol) were added to Et3N (8 mL). The solution was bubbled with N2 at rt for 5 min and then stirred at rt under N2 protection for 8 h. After the reaction was completed as checked by TLC analysis, the solvent was removed by rotary evaporation. The resulting residue was diluted with CHCl3. The mixture was filtered through a MgSO4 pad. The solution obtained was sequentially washed with HCl (aq 10%) and brine. The organic layer was dried over MgSO4 and concentrated under vacuum to give crude 53, which was further purified by silica flash column chromatography (hexanes/CH2Cl2, 7:3) to yield compound 53 (21 mg, 0.029 mmol, 28%) as a white solid. Mp 75-76 C; IR (KBr) 2920, 2872, 2852, 2203, 1692, 1600, 1581, 1568, 1514, 1499, 1466, 1418 cm-1; 1H NMR (CDCl3, 500 MHz) delta 10.68 (s, 1H), 8.08 (d, J=1.5 Hz, 1H), 7.70 (dd, J=8.5, 1.5 Hz, 1H), 7.50 (d, J=8.5 Hz, 2H), 7.49 (d, J=8.5 Hz, 2H), 7.02 (s, 1H), 7.01 (s, 1H), 6.90 (d, J=8.5 Hz, 1H), 4.06-4.02 (m, 4H), 3.85 (s, 3H), 1.90-1.84 (m, 4H), 1.59-1.47 (m, 4H), 1.42-1.27 (m, 24H), 0.90-0.87 (m, 6H); 13C NMR (CDCl3, 125 MHz) delta 191.3, 160.2, 154.7, 153.8, 137.4, 137.0, 134.5, 133.5, 130.5, 126.4, 123.3, 117.1, 116.5, 116.3, 115.8, 114.4, 112.1, 96.2, 95.0, 89.7, 85.0, 70.2, 69.7, 55.7, 32.3, 30.1, 30.05, 30.01, 30.0, 29.9, 29.8, 29.76, 29.70, 26.5, 23.1, 14.5; HRMS (CI) m/z calcd for C44H55BrO4 726.3284, found 727.3430 [M+H]+.

The synthetic route of 689291-89-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhou, Ningzhang; Wang, Li; Thompson, David W.; Zhao, Yuming; Tetrahedron; vol. 67; 1; (2011); p. 125 – 143;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 182056-39-9, These common heterocyclic compound, 182056-39-9, name is 2-Bromo-4-iodo-1-methoxybenzene, 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.

To a 100 ml round bottom flask was added copper (I) iodide (30.4 mg, 0.16 mmol), 2-(2-pyridyl)benzimidazole (31.2 mg, 0.16 mmol), cesium carbonate (625 mg, 1.92 mmol) and DMF (5.35 ml). The reaction mixture was heated to 60C for 1 h then (1 H-pyrazol-3-yl)methanol (235 mg, 2.40mmol) and 2-bromo-4-iodo-1-methoxybenzene (500 mg, 1.60 mmol) were added and the mixturewas heated at 1 oooc for 18 hours. The reaction was cooled, diluted with EtOAc and filteredthrough celite. The filtrate was concentrated in vacuo and purified by silica gel chromatography (0-1 00% EtOAc in Hepane) to afford (1-(3-bromo-4-methoxyphenyl)-1 H-pyrazol-3-yl)methanol (35310 mg) MS [M+2H+] = 285.0.

The synthetic route of 182056-39-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; CHEUNG, Atwood; CHIN, Donovan Noel; DALES, Natalie; FAZAL, Aleem; HURLEY, Timothy Brian; KERRIGAN, John; O’BRIEN, Gary; SHU, Lei; SUN, Robert; SUNG, Moo; WO2014/28459; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 401-81-0, 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.

General procedure: A Schlenk tube was charged with MCM-41-2N-CuI (66 mg,0.03 mmol), MeCSNH2(75 mg, 1.0 mmol), Cs2CO3(978 mg,3.0 mmol), and aryl halide (2.5 mmol). The tube was evacuated andbackfilled with argon. Then, DMSO-H2O (1 ml/0.5 ml) was addedunder argon. The tube was sealed, and the reaction mixture wasstirred at 120C for 24-48 h. The reaction mixture was cooled toroom temperature, diluted with ethyl acetate (10 ml), and filtered.The MCM-41-2N-CuI complex was washed with distilled water(2 × 5 ml), ethanol (2 × 5 ml), and Et2O (2 × 5 ml) and reused in thenext run. The filtrate was concentrated under reduced pressureand the residue was purified by flash column chromatography onsilica gel (petroleum/ethyl acetate = 50:1 to 7:1) to provide thedesired product.

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-3-(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Cai, Mingzhong; Yao, Ruiya; Chen, Lin; Zhao, Hong; Journal of Molecular Catalysis A: Chemical; vol. 395; (2014); p. 349 – 354;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 702641-04-1, The chemical industry reduces the impact on the environment during synthesis 702641-04-1, name is 2-Iodo-5-(trifluoromethyl)benzoic acid, I believe this compound will play a more active role in future production and life.

Borane-THF (1.0M solution in THF; 94 mL; 94 mmol) was added to a stirred solution of 2-iodo-5- (trifluoromethyl)benzoic acid (Intermediate 7, 2.97g; 9.4 mmol) in THF (300 mL) at O0C under N2- The reaction was heated at reflux for 90 min and then carefully quenched with 6N HCl until no further gas evolution. The reaction was diluted with H2O (250 mL) and extracted with EtOAc (3 x 250 mL). The combined extracts were washed with brine (300 mL), dried over MgSO-J, filtered, and concentrated in vacuo. The crude material was purified by flash chromatography on silica gel (0-25% EtOAc/hexanes gradient) to afford [2-iodo-5-(trifluoromethyl)phenyl]methanol as a white solid. LCMS = 285.0 (M – 17)+. lH NMR (CDCI3, 500 MHz): delta 7.97 (d, J= 8.3 Hz, 1 H), 7.79 (s, 1 H), 7.28 (d, J= 8.4 Hz, 1 H),4.75 (s, 2 H).

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, 2-Iodo-5-(trifluoromethyl)benzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2007/41494; (2007); A2;,
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. 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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
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. 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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com