Month: September 2021

Electric Literature 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;,
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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. 2106-04-9, name is 3-Chloro-2-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 3-Chloro-2-fluoroaniline

Step 64.2: 5-r(3-Chloro-2-fluoro-phenylamino)-(4-chloro-2-methyl-phenyl)-1-isopropyl-2-(2- methoxy-phenyl)-1 H-imidazole-4-carboxylic acid methyl ester Intermediate D (620 mg, 1.45 mmol) was dissolved in DCM (15 mL). TEA (366 mg, 0.5 mL, 3.61 mmol) and MsCI (331 mg, 2.90 mmol) were added and the reaction mixture was stirred at rt for 6 h. All volatiles were removed under reduced pressure and the residual crude mesylate re-dissolved in DCM (10 mL). 3-Chloro-2-fluoro aniline (310 mg, 2.13 mmol) was added and stirring continued at rt for 16h. The solvent was evaporated under reduced pressure. EtOAc (10 mL) and TEA (0.5 mL) were added and the mixture stirred for 5 min at rt. The white precipitate was filtered off and the filtrate concentrated to give the crude product which was purified by flash chromatography (heptanes/EtOAc, 100:0? 1 :1 ) to give the title compound. tR: 1.42 min (LC-MS 2); ESI-MS: 556.3/558.3 [M+H]+ (LC-MS 2).

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

Reference:
Patent; NOVARTIS AG; FURET, Pascal; GUAGNANO, Vito; HOLZER, Philipp; KALLEN, Joerg; LIAO, Lv; MAH, Robert; MAO, Liang; MASUYA, Keiichi; SCHLAPBACH, Achim; STUTZ, Stefan; VAUPEL, Andrea; WO2013/111105; (2013); A1;,
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Application of 4152-90-3,Some common heterocyclic compound, 4152-90-3, name is (3-Chlorophenyl)methanamine, molecular formula is C7H8ClN, 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 suspension of ethyl 6-brorno-4-hydroxyquinazoline-2-carboxylate (0.891 g, 3 rnrnol) and brornotri(pyrrolidin-1-yl)phosphoniurn hexafluorophosphate (2.10 g, 4.50 rnrnol) in 1,4-dioxane (12 rnl) was added Et3N (1.254 rnl, 9.0 rnrnol). The rnixture was stirred at rt for 3 h and then (3-chlorophenyl)rnethanarnine (0.85 g, 6.0 rnrnol) was added. The rnixture was stirred at rt for another 5 h. The rnixture was poured into hexane/H20 (10 rnL/10 rnL). The solid was filtered and triturated with 3percent EtOAc/hexane and then dried to give ethyl 6-brorno-4-((3- chlorobenzyl)arnino)quinazoline-2-carboxylate (1.2 g, 2.85 rnrnol, 95 percent yield). The rnaterial wasused without further purification. MS (M+H)= 421.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (3-Chlorophenyl)methanamine, its application will become more common.

Reference:
Patent; STROVEL, Jeffrey William; YOSHIOKA, Makoto; MALONEY, David J.; YANG, Shyh Ming; JADHAV, Ajit; URBAN, Daniel Jason; (334 pag.)WO2017/91661; (2017); A1;,
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Electric Literature of 883499-24-9,Some common heterocyclic compound, 883499-24-9, name is 1-Bromo-2-chloro-3-fluorobenzene, molecular formula is C6H3BrClF, 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.

In a nitrogen atmosphere, a flask containing 114 7-(diphenylamino)-9,9?-dimethyl-9H-fluoren-3-ol (100 g), 123 1-bromo-2-chloro-3-fluorobenzene (58.3 g), 77 potassium carbonate (91.5 g), and NMP (500 ml) was heated and stirred at a reflux temperature for four hours. After the reaction was stopped, the reaction liquid was cooled to room temperature, and 30 water was added thereto. A precipitate thus precipitated was collected by suction filtration. The obtained precipitate was washed with water and then with methanol and then purified by silica gel column chromatography (eluent: toluene) to obtain an intermediate 124 6-(3-bromo-2-chlorophenoxy)-9,9-dimethyl-N,N-diphenyl-9H-fluoren-2-amine (150 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2-chloro-3-fluorobenzene, its application will become more common.

Reference:
Patent; JNC CORPORATION; FUJITA, Yukihiro; (228 pag.)US2019/165279; (2019); A1;,
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These common heterocyclic compound, 106-39-8, name is 1-Bromo-4-chlorobenzene, 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. Recommanded Product: 106-39-8

General procedure: To a round bottle with a magnetic stir bar, ligand (0.01% mmol), PdCl2 (0.01% mmol), aryl halides (1.0 mmol), phenylboronic acid (1.2 mmol), K2CO3 (2.0 mmol) and 6 ml of solvent were added. The reaction mixture was conducted at room temperature for the required time, and then the solvent was removed under reduced pressure. The residual was diluted with Et2O (5 mL), followed by extraction twice (2×5 mL) with Et2O. The organic layer was dried with anhydrous MgSO4, filtered and evaporated under vacuum. The conversions rates were analyzed by gas chromatography, based on the peak area normalization method. The corrected factor was determined by samples against a standard of n-heptane. The crude products were purified by silica-gel column chromatography using petroleum ether-ethyl acetate (20:1) as an eluent, and the isolated yield was then calculated based on the feeding of the aryl halide. The isolated corresponding products were characterized by 1H NMR and 13C NMR.

The synthetic route of 1-Bromo-4-chlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhou, Zhen; Cao, Gao; Liu, Ning; Chemistry Letters; vol. 48; 6; (2019); p. 547 – 550;,
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Adding a certain compound to certain chemical reactions, such as: 81927-55-1, name is Benzyl 2,2,2-trichloroacetimidate, 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 81927-55-1, Product Details of 81927-55-1

To a solution of (R)-Roche ester 25 (200 mg, 1.69 mmol, 1equiv) in CH2Cl2 (3 mL) was added at 0 oC benzyl trichloroacetimidate (640 mg, 2.54 mmol, 1.5 equiv). Asolution of CF3SO3H in CH2Cl2 (0.85 M, 100 muL, 0.09 mmol, 0.05 equiv) was added at 0 oC and the mixture wasstirred at room temperature for 44 h. After filtration, the filtrate was concentrated under reduced pressureand saturated aqueous NaHCO3 (15 mL) was added. The aqueous layer was extracted with EtOAc, thecombined organic layers were washed with brine, dried over MgSO4 and concentrated under reducedpressure. The crude mixture was purified by flash column chromatography (SiO2, petroleum ether/Et2O: 95/5)to afford the desired product 26 (262 mg, 74%) as a yellow oil. Rf (cyclohexane/EtOAc: 9/1, UV, KMnO4) 0.30;-8.0 (c 1.60, CHCl3); 1H NMR (CDCl3, 300 MHz) delta = 7.38 – 7.24 (m, 5H), 4.53 (s, 2H), 3.70 (s, 3H), 3.66 (dd,J 9.2, 7.3 Hz, 1H), 3.50 (dd, J 9.1, 5.9 Hz, 1H), 2.86 – 2.72 (m, 1H), 1.18 (d, J 7.1 Hz, 3H); 13C NMR (CDCl3, 75MHz) delta 175.4, 138.3, 128.5, 127.7 (2C), 73.2, 72.1, 51.8, 40.3, 14.1

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, Benzyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Echeverria, Pierre-Georges; Pons, Amandine; Prevost, Sebastien; Ferard, Charlene; Cornil, Johan; Guerinot, Amandine; Cossy, Janine; Phansavath, Phannarath; Ratovelomanana-Vidal, Virginie; Arkivoc; vol. 2019; 4; (2019); p. 44 – 68;,
Chloride – 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. 7781-10-4, name is 4-Chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine, A new synthetic method of this compound is introduced below., COA of Formula: C7H6ClN3

General procedure: P-aminophenol or 2-fluoro-4-aminphenol 18a-b (0.1 mol)whichwas dissolved in tetrahydrofuran (50 ml),was added to a 1,4-dioxane/H2O(50 ml, 5:1) solution of compounds 17a-b or 20a-b,sodium carbonate and hydrogen sodium at 80 C for 2 h. Then thesolution was concentrated in vacuum and washed with water,filtered to give a solid.

The synthetic route of 7781-10-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Lin Xiao; Liu, Xiaobo; Xu, Shan; Tang, Qidong; Duan, Yongli; Xiao, Zhen; Zhi, Jia; Jiang, Liwen; Zheng, Pengwu; Zhu, Wufu; European Journal of Medicinal Chemistry; vol. 141; (2017); p. 538 – 551;,
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Synthetic Route of 2162-98-3,Some common heterocyclic compound, 2162-98-3, name is 1,10-Dichlorodecane, molecular formula is C10H20Cl2, 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 8 20.6 g (0.1 mol) of 4-octylaminopyridine, 10.5 g (0.05 mol) of 1,10-dichlorodecane and 30 ml of white spirit (boiling point 155 to 200 C.) were combined and heated to 130 C. The exothermic reaction causes the temperature to increase to 155 C., and at the same time white crystal precipitate out. The reaction mixture was stirred for a further 4 hours at 140 C., and after cooling to room temperature the very fine crystal sludge was filtered over a filterpaper and washed with petroleum ether, giving a beige, solid mass. The reaction product octenidine dihydrochloride in this example is very difficult to filter off with suction since it is produced in very fine form.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,10-Dichlorodecane, its application will become more common.

Reference:
Patent; AIR LIQUIDE SANTE (INTERNATIONAL); US2001/16660; (2001); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 20850-43-5, 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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows.

Taking 10 g about 89.7% content piperazine pyrimidine, 12 g triethylamine, 34 ml isopropanol into 100 ml three port into reaction, stirring at the room temperature under the chlorosilane dropping pepper, in 30 minutes in the transfusion. Heating to 50 C, thermal insulation 4 hours, stirring under cooling to room temperature, filter, recovery mother liquor, in the filter cake by adding 20 ml water beating, filtering, adding 10 ml water washes filters cake. 50 C drying, the crude product shall piribedil 16.6 g, HPLC analysis content 99.2%. Yield 92%

The chemical industry reduces the impact on the environment during synthesis 5-(Chloromethyl)benzo[d][1,3]dioxole. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Taicang Hongshan Environmental Protection Technology Co., Ltd.; Liu Lu; (9 pag.)CN107216318; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 60811-18-9, 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. 60811-18-9, name is 4-Bromo-1-chloro-2-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(7) Metal magnesium in an amount of 12 g was suspended in 10 ml of THF under nitrogen gas stream, and a solution prepared by dissolving 10.3 g of 3-fluoro-4-chloro-bromobenzene in 50 ml of THF was added dropwise thereto and stirred at room temperature for 1 hour to prepare a solution of Grignard reagent. In 50 ml of THF was dissolved 10.6 of the 4-(2-(trans-4-(2-(4-n-propylphenyl)ethyl)cyclohexyl)ethyl)iodobenzene, and 1 g of palladium chloride was added thereto and stirred under a reflux. The solution of Grignard reagent prepared in the previous procedures was added dropwise thereto and reacted while stirring for 2 hours. Reaction solution thus obtained was added to 200 ml of dilute hydrochloric acid, and the product was extracted with 200 ml of heptane. Organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain a yellow-brown oily product. This product was purified by a column chromatography over an alumina by using heptane as an eluent, and further recrystallized from heptane to obtain 2 g of the subject compound. According to the procedures mentioned above, the following Compounds No. 128 to 189 were synthesised:

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, 4-Bromo-1-chloro-2-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chisso Corporation; US5858275; (1999); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics