Month: March 2021

Application of 1939-99-7, These common heterocyclic compound, 1939-99-7, name is Phenylmethanesulfonyl chloride, 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.

Preparation 19: 3-Phenyl-l ,4,5-oxathiazepane 4,4-dioxide Step 1 : A/-(2-((Tert-butyldimethylsilyl)oxy)ethyl)- 1 -phenylmethanesulfonamide To a solution of 2-((tert-butyldimethylsilyl)oxy)ethanamine (11.7 g, 66.6 mmol) and triethylamine (11.2 mL, 79.9 mmol) in tetrahydrofuran (222 mL) at 0 C was slowly added phenylmethanesulfonyl chloride (12.7 g, 66.6 mmol) portion wise and the reaction was stirred at room temperature for 16 hours. MTBE was then added and the Et3N HCl salt was removed by filtration. The filtrate was then concentrated and purified by silica gel solumn chromatography (0-30% Acetone in heptane, 216 nM) to A^-(2-((tert-butyldimethylsilyl)oxy)ethyl)-l-phenylmethanesulfonamide (17.8 g, 81 % yield). LCMS (ESI), m/z, 330. [M+H] +.

The synthetic route of 1939-99-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; FAUBER, Benjamin; LADDYWAHETTY, Tammy; RENE, Olivier; (105 pag.)WO2016/96936; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 29671-92-9, name is Carbamimidic chloride hydrochloride, A new synthetic method of this compound is introduced below., Computed Properties of CH4Cl2N2

To a suspension of Ig (400 mg, 0.66 mmol) in methanol (26 mL) was dropwise added concentrated HCl (4.5 mL) while stirring. The mixture was stirred at room temperature for 1 h. The resulting solution was concentrated in vacuo and dried. The residue was then mixed with methyl sulfone (6 g) and chloroamidine hydrochloride (113 mg, 0.99 mmol) in a microwave vial, and heated at 150 0C for 1 h. While cooling to room temperature, the mixture was treated with IN ammonium hydroxide (5 mL) and ethyl acetate (5 mL) with vigorous stirring. The organic layer was concentrated and the residue was purified by silica gel column chromatography (EtOAc / hexanes), affording 3a as an oil (0.05 g, 13%). MS = 584.0 (M+ H+). 1H NMR (300 MHz, CDCl3): B 8.09 (s, IH), 7.2-7.4 (m, 15H), 5.33 (s, IH), 4.4-4.8 (m, 7H), 3.96 (m, IH), 3.86 (m, 2H), 1.16 (s, 3H).

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; GILEAD SCIENCES, INC.; BUTLER, Thomas; CHO, Aesop; KIM, Choung, U.; XU, Jie; WO2010/93608; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 363-51-9, name is 2-Chloro-6-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2-Chloro-6-fluoroaniline

A stirred solution of 9 4-hydroxy-2-methylsulfanyl-pyrimidine-5-carboxylic acid (5.70 g, 30.65 mmol, 1.0 eq) and 237 2-chloro-6-fluoro-aniline (4.50 g, 30.65 mmol, 1.0 eq) in 24 toluene (200 mL) was purged with nitrogen gas for 15 min. To the above solution 91 PCl3 (30 mL) was added. The reaction was heated at 100 C. for 72 h. Progress of reaction was monitored by LCMS. After completion of reaction, solvent was removed under reduced pressure, residue was diluted with a mixture of 238 diethyl ether: 30 MeOH (10:1) (100 mL) stirred for 15 min then filtered off. Solid was suspended in MeOH (20 mL), stirred for 5 min, filtered off and washed with MeOH (10 mL), and then dried under vacuum to obtain of 239 N-(2-chloro-6-fluoro-phenyl)-4-hydroxy-2-methylsulfanyl-pyrimidine-5-carboxamide (5.0 g, 52.8%). (0370) LCMS: 314 [M+1]+

The synthetic route of 363-51-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; giraFpharma LLC; Chakravarty, Sarvajit; PHAM, Son Minh; Kankanala, Jayakanth; AGARWAL, Anil Kumar; PUJALA, Brahmam; SONI, Sanjeev; ARYA, Satish K.; PALVE, Deepak; KUMAR, Varun; (360 pag.)US2019/106436; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 93-50-5, name is 4-Chloro-2-methoxyaniline, belongs to chlorides-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 93-50-5, SDS of cas: 93-50-5

To a solution of 4-chloro-2-methoxy-phenylamine (600 mg, 3.81 mmol) in ethanol (12 ml) at 50C was added a solution of silver sulphate (2.14 g, 6.85 mmol) and iodine (967 mg, 3.81 mmol) in ethanol (8 ml). The resulting reaction mixture was stirred at 50C for 4h. After cooling at 25C, reaction mixture was filtered through a bed of celite and the filtrate was diluted with EtOAc (30 ml). The organic phase was washed with aqueous Na2S203 solution (2×15 ml), and brine (10 ml), dried over anhydrous Na2S04, filtered, and evaporated off in vacuo. The crude residue was purified by flash column chromatography (2% EtOAc in hexane) to afford 4-chloro-2-iodo-6-methoxy-phenylamine (160mg, 15%) as brown sticky liquid. GC-MS: 283 (M).

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; F. HOFFMANN-LA ROCHE AG; CECCARELLI, Simona M.; CONTE, Aurelia; KUEHNE, Holger; KUHN, Bernd; NEIDHART, Werner; OBST SANDER, Ulrike; RUDOLPH, Markus; WO2013/64465; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, belongs to chlorides-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 33863-76-2, COA of Formula: C6H3BrClF

A solution of 1-bromo-3-chloro-5-fluorobenzene (50.0 g, 239 mmol) in DMF (300 ml.) was treated with sodium methoxide (15.5 g, 286 mmol) and the reaction was stirred overnight at rt. The mixture was diluted with ethyl acetate (500 ml.) and washed with water (700 ml_). The organic layer was isolated, washed with brine, dried over magnesium sulfate, filtered, and concentrated to give 51.0 g of the title compound which was used without purification. 1H NMR (DMSOd6) ¡ì 7.23 (t, 1 H), 7.13 – 7.15 (m, 1 H), 7.05 (t, 1 H), 3.77 (s, 3 H).

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; SMITHKLINE BEECHAM CORPORATION; WO2008/157330; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 622-24-2, 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 622-24-2 as follows.

To the reaction flask was added substances five, six substances, dimethylformamide, potassium carbonate, the reaction was cooled to 25 , the reaction mixture was added to ice water, ice-water is 10 times the mass of the reaction liquid was filtered, washed with water, Dry matter seven. The molar ratio of the substance five, substance six, potassium carbonate and dimethylformamide was 1: 1: 1: 10, and the temperature was raised to 80 C for 4 hours

According to the analysis of related databases, 622-24-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CHINA THREE GORGES UNIVERSITY; TAN, XIAO; LIU, SEN; YANG, LITING; (22 pag.)CN106243058; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., SDS of cas: 63624-28-2

B) 5-Chloro-3-(2-isopropoxyphenyl)-1-[(2,4-dimethoxyphenyl)sulphonyl]-3-[2-oxo-2-[4-(4-pyridyl)-1-piperazinyl]ethyl]-1,3-dihydro-2H-indol-2-one, laevorotatory isomer. 0.025 g of 60% sodium hydride in oil is added to a mixture of 0.3 g of the compound obtained in the preceding step in 10 ml of THF, and the mixture is stirred at 20 C. for 15 minutes. 0.19 g of 2,4-dimethoxybenzenesulphonyl chloride is then added and the mixture is stirred at 20 C. for 2 hours.The reaction mixture is concentrated under vacuum, the residue is taken up in water and extracted with EtOAc, the organic phase is dried over Na2SO4 and the solvent is evaporated off under vacuum.The residue is chromatographed on silica gel, eluding with DCM and then with acetone. 0.1 g of the expected product is obtained. 1H NMR: DMSO-d6: delta (ppm): 0.6: d: 3H; 1.2: d: 3H; 3.0 to 4.0: m+2s: 16H; 4.6: mt: 1H; 6.4 to 7.2: mt: 9H; 7.4: bd: 1H; 7.7: dd: 2H; 8.1: d: 2H.

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; Di Malta, Alain; Garcia, Georges; Roux, Richard; Schoentjes, Bruno; Serradeil-Le Gal, Claudine; Tonnerre, Bernard; Wagnon, Jean; US2004/180878; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2106-04-9, These common heterocyclic compound, 2106-04-9, name is 3-Chloro-2-fluoroaniline, 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.

Sodium nitrite (9.7 g, 0.14 mol) was dissolved in 25 mL of water and added to the solution cooled to -5 C.3-chloro-2-fluoroaniline (20.0 g, 0.14 mmol) in trifluoroacetic acid (100 mL),Sodium azide (9.1 g, 0.14 mol) dissolved in 5 mL of water was added dropwise to the reaction solution, and the mixture was dropped.The reaction mixture was stirred at 0 C for 2 hr then quThe organic phase is dried and filtered.After concentration, the title compound (18.7 g) was obtained.Used directly in the next step.

The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Wu Yongyong; Song Zhiquan; Cai Jiaqiang; Zhu Jiawang; Wang Lichun; Wang Jingyi; (71 pag.)CN109867660; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2770-11-8,Some common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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 stirred and cooled solution of 2-(4-chlorophenoxy)aniline (330 mg, 1.50 mmol) and triethylamine (230 muL, 1.65 mmol) in toluene (5 mL), the appropriate acid chloride (pivaloyl chloride, 2,2-dimethylbutyryl chloride, 3-methylbutyryl chloride, propyl chloride, cyclopropanecarbonyl chloride, cyclobutanecarbonyl chloride, methyl succinyl chloride, 4-methoxybenzoyl chloride) (1.65 mmol) was added. Subsequently the reaction mixture was allowed to warm to room temperature. The progress of the reaction was monitored by TLC. After 2-9 h the reaction mixture was extracted with a saturated sodium hydrogen carbonate solution, with a hydrogen chloride solution (10%), with brine and finally with water. Afterwards the organic solution was dried over sodium sulfate and evaporated under reduced pressure. The residue was further purified by recrystallization or column chromatography over silica gel.

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

Reference:
Article; Weidner, Thomas; Nasereddin, Abed; Preu, Lutz; Gruenefeld, Johann; Dzikowski, Ron; Kunick, Conrad; Molecules; vol. 21; 2; (2016);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 2732-80-1, 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. 2732-80-1, name is 2-Bromo-1-chloro-4-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

The 2-bromo-1-chloro-4-methoxybenzene (25.0 g, 113 mmol) [Oakwood cat035670] was dissolved in carbon disulfide (250 mL), and the acetyl chloride (12 mL, 170 mmol) and aluminum trichloride (37.6 g, 282 mmol) were added. The reaction was heated to reflux and monitored by LC/MS. After heating for 1 h, the reaction became two layers. The reaction allowed to cool to room temperature and poured over ice. The slurry was extracted with ethyl acetate 3¡Á, the combined organic layer was washed with brine, dried over magnesium sulfate and concentrated to give 1-(4-bromo-5-chloro-2-hydroxyphenyl)ethanone as a solid (28.0 g, 99%). 1H NMR (300 MHz, CDCl3) delta 12.12 (s, 1H), 7.78 (s, 1H), 7.31 (s, 1H), 2.62 (s, 3H).

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-1-chloro-4-methoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Combs, Andrew P.; Sparks, Richard B.; Maduskuie, Jr., Thomas P.; US2013/261101; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics