Month: November 2020

Adding a certain compound to certain chemical reactions, such as: 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, 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 915095-86-2, 915095-86-2

5-Iodo-2-chloro-4′-fluorobenzophenone (V-2) (18.5 g, 0.051 mol) was dissolved in 50 ml of tetrahydrofuran solutionThen, (5)-3_light-based tetrahydrofuran (4.9 g, 0.056 mol) was added and stirred, and finally a solution of potassium t-butoxide (6.9 g, 0.061 mol) dissolved in 30 ml of tetrahydrofuran was added dropwise, and the temperature was controlled at 16-25 ¡ã C. After the addition was completed, the reaction was stirred at 20 ¡ã C for 1 hour, and the reaction was almost complete by TLC, and the purified water was slowly added and stirred for 30 min.The solution was separated and the organic phase was dried. After column chromatography, 14. lg (64.3percent) of solid was obtained.

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-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Huarun Shuang He Pharmaceutical Co., Ltd.; Zhai Jianguo; He Yang; Zhu Yingjie; Zhou Yisui; Ma Hongmin; Song Meng; (46 pag.)CN108218928; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

1878-69-9, Adding a certain compound to certain chemical reactions, such as: 1878-69-9, name is 2-(3-Iodophenyl)acetic acid, 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 1878-69-9.

To a suspension of 2-(2-Amino-5-ethynyl-pyrimidin-4-yl)-1-methyl-4-oxo-1 ,4,6,7 -tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester (1.56 g, 4.25 mmol) in degassed MeCN (25 ml), Cui (1 0% mol, 81 mg, 0.425 mmol),3-iodophenylacetic acid (1.17 g, 4.25 mmol), TEA (5.92 ml, 42.48 mmol) and PdCb(PPh3)2 (1 0% mol, 0.30 g, 0.425mmol) were added. The mixture was degassed for three times back filling with argon each time and let under stirring5 at r.t. for 1 h. The reaction was quenched with 2 N HCI (21.2 ml) and the solvent was removed under reducedpressure. The residue was suspended in water and the resulting solid was filtered and rinsed with water affording thetitle product and brownish solid (1.62 g, 76%).(ESI) m/z 502 [(M +H)+]. HRMS (ESI) calculated for C21H2sN505 [(M + H)+]502.2085; found 502.2074.

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-(3-Iodophenyl)acetic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NERVIANO MEDICAL SCIENCES S.R.L.; MENICHINCHERI, Maria; ANGIOLINI, Mauro; BERTRAND, Jay Aaron; CARUSO, Michele; POLUCCI, Paolo; QUARTIERI, Francesca; SALOM, Barbara; SALSA, Matteo; ZUCCOTTO, Fabio; WO2014/72220; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

Step 7. N-(1,1-difluoro-2,3-dihydro-3-(4-methylpiperazin-1-yl)-1H-indan-6-yl)-3-iodo-4-methylbenzamide A solution of 3-iodo-4-methylbenzoic acid (79 mg, 0.3 mmol) in SOCl2 (5 mL) was refluxed for 3 h, then evaporated in vacuum to remove residual SOCl2. The residue was dissolved in 5 mL anhydrous THF and added to a solution of triethylamine (37 mg, 0.36 mmol), 1-(1,1-Difluoro-2,3-dihydro-6-amino-1H-indan-3-yl)-4-methylpiperazine (78 mg, 0.3 mmol) and DMAP (2 mg) in 5 mL anhydrous THF in dropwise. The result mixture was stirred at rt for 26 h, and evaporated in vacuum. The residue was purified by chromatography on silica gel (CH2Cl2/CH3OH 97:3) to give 140 mg product as a pale yellow solid (91.5%). LCMS: m/z [M+H]+ 512.1049.

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; Astar Biotech LLC; YU, Chunrong; Huang, Haihong; Zhang, Dongfeng; Li, Peng; US2014/31354; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 624-75-9, name is 2-Iodoacetonitrile, 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 624-75-9, 624-75-9

Example 41 Benzyl {(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro-[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}(cyanomethyl)carbamate Potassium carbonate (15.7 mg, 113 mmol, 2.1 eq.), 18-crown-6 (30 mg, 113 mmol, 2.1 eq.) and iodoacetonitrile (19 mg, 113 mmol, 2.1 eq.) were added to a solution of benzyl {(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}carbamate (30 mg, 54 mmol) in DMF (2 ml). The reaction mixture was stirred at RT for 12 h and then concentrated under reduced pressure. The residue was acidified with acetic acid and then purified by preparative HPLC (Kromasil C18 column, 5 mum, 50*20 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (25 mg, 78% of theory). LC-MS (Method 5): Rt=1.40 min; MS (ESIpos): m/z (%)=434.0 (100), 550.9 (20), 595.0 (30) [M+H]+; MS (ESIneg): m/z (%)=593.8 (100) [M-H]-. 1H-NMR (400 MHz, DMSO-d6): delta=2.00 (s, 3H), 4.55 (d, 2H), 5.10 (d, 2H), 6.55 (s, 1H), 7.15-7.35 (m, 5H), 7.70-7.95 (m, 7H), 8.15 (br. s, 1H).

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-Iodoacetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; US2012/4203; (2012); 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., 3058-39-7

General procedure: A 50 mL round-bottomed flask, equipped with a gas inlet tube, a refluxcondenser and a magnetic stirring bar was charged with MCM-41-2PPdCl2 (102 mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa(7.5 mmol). The flask was flushed with CO. DMF (5 mL) was addedby syringe and a slow stream of CO was passed into the suspension.The mixture was vigorously stirred at 110?130 ¡ãC for 2?20 h, cooledto room temperature and diluted with diethyl ether (50 mL). Thepalladium catalyst was separated from the mixture by filtration,washed with distilled water (2 ¡Á 10 mL), ethanol (2 ¡Á 10 mL) and ether(2 ¡Á 10 mL) and reused in the next run. The ethereal solution waswashed with water (3 ¡Á 20 mL), and dried over anhydrous magnesiumsulfate and concentrated under reduced pressure. The residue waspurified by flash column chromatography on silica gel (hexane?ethylacetate = 10 : 1).

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:
Article; Jiang, Jianwen; Wang, Pingping; Cai, Mingzhong; Journal of Chemical Research; vol. 38; 4; (2014); p. 218 – 222;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 612-55-5, name is 2-Iodonaphthalene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 612-55-5

An appropriate amount of DMF was added to the reaction vessel and purged with nitrogen until the atmosphere was a nitrogen atmosphere. Then 100 mmol of the compound of the above formula (II), 200 mmol of the compound of the above formula (III)7 mmol of bis (triphenylphosphine) cuprous nitrate,100 mmol DABCO and 15 mmol promoter (a mixture of 13 mmol triethyloxonium tetrafluoroborate and 2 mmol AgBF4), warmed to 100 C and reacted at this temperature for 12 hours.After completion of the reaction, saturated brine was added to sufficiently wash the organic phase, the organic phase was separated, washed thoroughly with deionized water and extracted with ether. The upper organic layer was taken, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was passed through a silica gel column Chromatography. The eluent used for column chromatography was a mixture of chloroform and petroleum ether. The volume ratio of the two was 1: 3 to obtain the compound of formula (I). The yield was 95.6%

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, 612-55-5, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wuhan Jinlian Pharmaceutical Co., Ltd.; Dong Xiao; Jin Yunhe; Lu Jun; Zhu Benfa; (10 pag.)CN104529854; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common heterocyclic compound, 624-75-9, name is 2-Iodoacetonitrile, molecular formula is C2H2IN, 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. 624-75-9.

To a mixture of 5-bromo-2-isopropyl-4-methoxy-phenol from step 4 (0.831 g, 3.4 mmol) and K2CO3 (0.562 g, 4.1 mmol) in 17 mL dimethyl formamide (DMF) was added iodoacetonitrile (0.594 g, 3.6 mmol). The mixture was warmed to 60 C. for 30 minutes and then allowed to cool to room temperature. After cooling to room temperature the mixture was taken up in 50 mL of H2O and extracted with 1:1 toluene/ethyl acetate, washed with H2O and then with brine. The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo to give a crude solid. Purification via flash chromatography (1:1 hexane/CH2Cl2) afforded (5-bromo-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (0.611 g, 63%) as a while solid.

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

Reference:
Patent; Roche Palo Alto LLC; US2007/49609; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, 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. 83863-33-6

In a 10 mL round-bottomed flask was dissolved 5-iodo-2-methylaniline (5.171 g, 22.19 mmol), 4-(pyridin-2-ylmethoxy)benzoic acid, HCl (4.91 g, 18.49 mmol), DIPEA (9.66 mL, 55.47 mmol) and HATU (14.06 g, 36.98 mmol) in NMP (92 mL) to give an orange solution. The reaction was heated to 70 0C for 12h, after which time, the reaction was poured into IM aqueous NaOH (400 mL), and the resultant precipitate was removed via vacuum filtration. The filter cake was rinsed with water (200 mL), MTBE (100 mL), and dried under suction to yield the title compound (5.52 g, 67%) as a pale brown solid. 1H NMR (DMSO-d6) delta 2.19 (s, 3 H) 5.29 (s, 2 H) 7.08 (d, 1 H) 7.16 (m, 2 H) 7.29 – 7.43 (m, 1 H) 7.50 (dd, 1 H) 7.55 (d, 1 H) 7.73 (d, 1 H) 7.87 (td, 1 H) 7.95 (m, 2 H) 8.61 (d, 1 H) 9.78 (s, 1 H). MS (M+H+) = 445.

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 83863-33-6.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2009/27746; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

5471-81-8, Adding a certain compound to certain chemical reactions, such as: 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, 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 5471-81-8.

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),Nitrogen protection (at least three nitrogen cycles), followed by a mixture of acetonitrile and N,N-dimethylformamide in a nitrogen stream (V/V=1, 3 ml)And methyl 4-iodo-3-methylbenzoate (99.4 mg, 0.36 mmol), closed vessel.The reaction solution was heated to 80 C. for about 12 h, and the reaction was complete by TLC.In the post-treatment, the reaction solution is first diluted with 15 ml of ethyl acetate, and then filtered through a sand funnel filled with silica gel.Remove inorganic substances such as catalysts and alkalis,The resulting filtrate was separated by flash column chromatography to give the pure product 5,7-dimethyldibenzo[c,e][1,2]thiazine-9-carboxylic acid methyl ester-5-oxide compound 3m. Yield: 87%.

According to the analysis of related databases, 5471-81-8, the application of this compound in the production field has become more and more popular.

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

4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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: 4-Iodoanisole (1mmol), TMSA (1.1mmol) and K2CO3 (2mmol) were added to a freshly prepared solution of PdNPs (5mL) in a 25mL round bottomed flask fitted with stopper. Then, the reaction mixture was stirred at 40¡ãC. The reaction progress was monitored by TLC, until complete consumption of aryl iodide. To the reaction mixture containing in situ formed 4-ethynylanisole the next batch of aryliodide (1mmol) was added and the reaction mixture was further allowed to stir until complete consumption of the arylacetylene. In this manner the targeted unsymmetrical diarylacetylene was formed. The detailed procedure is provided in the Supp. Info. Detailed procedure for synthesis of symmetrical diarylacetylenes is also mentioned in SI.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Mandali, Pavan Kumar; Chand, Dillip Kumar; Catalysis Communications; vol. 47; (2014); p. 40 – 44;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com