Month: September 2021

Application of 33353-68-3, 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. 33353-68-3, name is 3,5-Dichloro-2-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 67D (0.5 g, 1.42 mmol)And 3,5-dichloro-2-methoxyaniline (0.3 g, 1.56 mmol) was dissolved in 10 mL of N,N-dimethylformamide, and sodium iodide (0.1 g, 0.71 mmol) was added.And potassium carbonate (0.59 mg, 4.3 mmol).The reaction system was heated to 90 C for 1 h, and LCMS showed the reaction was completed.Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The solvent was dried under reduced pressure.Column chromatography purification (ethyl acetate / petroleum ether = 1 / 50 ~ 1 / 30)The yellow solid compound 67E (0.16 g, 45% yield) 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, 3,5-Dichloro-2-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Xiansheng Pharmaceutical Co., Ltd.; Chen Huanming; Liang Bo; Cao Wenjie; Zhang Guiping; Zhao Zhongqiang; Jiang Zhaojian; Zuo Gaolei; Xu Wanmei; Gong Hongju; Zhang Peng; Wang Jianghuai; Li Qingsong; Gao Chunhua; (79 pag.)CN104045552; (2019); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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 94-97-3, 94-97-3

A mixture of 5-chloro-1H-benzotriazole (8 g), chloroacetone (6.5 mL), potassium carbonate (9.5 g) and potassium iodide (0.5 g) was stirred in acetone (90 mL) at room temperature for 48 hours. The reaction mixture was filtered and the filtrate concentrated under reduced pressure to give a residue that was purified by chromatography (SiO2, heptane/EA) to afford 1-(5-chloro-2H-benzotriazol-2-yl)-propan-2-one as clear oil [1.8 g, 16%, Rf=0.6 (1:1 EA/heptane)]. The two other regioisomers were also isolated, 1-(6-chloro-1H-benzotriazol-1-yl)-propan-2-one [3.8 g, 35%, Rf=0.45 (1:1 EA/heptane)] and 1-(5-chloro-1H-benzotriazol-1-yl)-propan-2-one [3.2 g, 29%, Rf=0.35 (1:1 EA/heptane)].

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, 5-Chloro-1H-benzo[d][1,2,3]triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Soll, Mark David; Hir de Fallois, Loic Patrick Le; Huber, Scot Kevin; Lee, Hyoung Ik; Wilkinson, Douglas Edward; Jacobs, Robert Toms; Beck, Brent Christopher; US2010/125089; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 6940-78-9, name is 1-Bromo-4-chlorobutane, molecular formula is C4H8BrCl, 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: C4H8BrCl

Example (C):1Preparation of 7-(4-cMorobutoxy)-3,4-dihydro carbostyril (III):; The three necked flask was charged with 7-hydroxy-3, 4-dihydro carbostyril (II) (50gm, 0.306moles) in acetone: water mixture (400ml: 25ml). To this mixture was successively added potassium carbonate (50,8gm, 0,367moles), PEG-400 (61.2gm) and stirred at ambient temperature for one hour. The l-bromo-4-chlorobutane (157ml, 0.918moles) was added to mixture over a period of 10 min. Reaction mixture was then stirred at ambient temperature for 15-16 hours. The progress of the reaction was monitored by TLC (eluent: chloroform: methanol (90:10)). Reaction mixture was filtered and the inorganics were washed with acetone (100ml). The solvent was removed under the reduced pressure below 40 0C. The thick oily residue obtained was stirred with n-hexane (500ml) and water (500ml), at 10-15 0C, for a period of 45 min.The solid was filtered, washed with water (500ml) and then with n-hexane (500ml). The resulting solid was dried at 65-70 0C to obtain 7-(4-chlorobutoxy)-3, 4-dihydro carbostyril (III) (72.7gm, 94 %).1H (CDCl3): 1.9 (m, 4H), 2.5 (m, 2H), 2.8 (m, 2H), 3.6 (m, 2H), 3.9 (m, 2H), 6.3 (s, IH), 6.4 (d, IH), 7.0 (d, IH) and 9.3 (s, IH)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6940-78-9, its application will become more common.

Reference:
Patent; UNICHEM LABORATORIES LIMITED; WO2007/94009; (2007); 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. 2163-00-0, name is 1,6-Dichlorohexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1,6-Dichlorohexane

A 250 mL four-necked flask equipped with a mechanical stirrer, a thermometer and a reflux condenser was used as the reaction vessel. 32. 3 g (0.13 mol) of sodium thiosulfate pentahydrate was weighed out, 70.0 g of water and 35. 0 g of DMF were added, After stirring and dissolving, 9.3 g (0.06 mol) of 1,6-dichlorohexane was added while stirring. The temperature of the solution was raised by heating, and the temperature of the reaction solution was raised to 90 C. The reaction was stirred at this temperature for 6 h, Hexamethylene-1,6-dithiosulfate disodium salt (HTS) solution. The resulting hexamethylene-1,6-dithio-sulfate disodium salt solution was analyzed by a gas chromatograph (GC) and a liquid chromatograph (HPLC), respectively, to measure 1,6-dichlorohexane and thiosulfate Sodium in the solution

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Red Avenue Innova Co., Ltd; Zhen, Boming; Dong, Dong; Zhao, Lili; fang, Caiqin; Ruan, zhen Gang; Hu, Xiaona; (10 pag.)CN105218419; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1303587-99-6, name is 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine, 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 1303587-99-6, Formula: C6H6ClN3O

Synthesis of2-chloro-8-(2, 2, 2-trifluoroethyl)-7, 8-dihydro-6H-pyrimido [5, 4-b] [I, 4] oxazine [0414] To a stirred solution of 2-chloro-7, 8-dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (500 mg, 2.92 mmol) in DMF (5 mL) under argon atmosphere were added cesium carbonate (1.9 g, 5.84 mmol) and 1, 1, l-trifluoro-2-iodoethane (611 mg, 2.92 mmol) at RT and the mixture was stirred for 32 h. After consumption of the starting materials (monitored by TLC), the reaction was diluted with water (20 mL) and extracted with EtOAc (2 x 20 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by silica gel column chromatography using 20% EtOAc:hexanes to afford 2-chloro-8-(2, 2, 2-trifluoroethyl)-7, 8-dihydro-6H-pyrimido [5, 4- b] [1, 4] oxazine (235 mg, 32%) as an off-white solid. 1H-NMR (CDC13, 500 MHz): delta 7.79 (s, 1H), 4.30-4.28 (m, 2H), 4.27-4.23 (m, 2H), 3.70-3.68 (m, 2H); LC-MS: 254.4 (M+1); (column; X-Select CSH C-18 (50 3.0 mm, 3.5 mupiiota); RT 3.76 min. 0.05% Aq TFA: ACN; 0.80 mL/min); TLC: 60% EtOAc:hexanes (R/. 0.6).

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; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H7ClFN

To a stirred mixture of 1-(2-chloro-4-fluorophenyl)methanamine (80 mg, 0.501 mmol, 1 equiv.) and 4-chloro-5-(4-oxopiperidin-1-yl)-2,3-dihydropyridazin-3-one (114.12 mg, 0.501 mmol, 1.00 equiv.) in DMF (5 mL) were added 1-azido-4-nitrobenzene (115.18 mg, 0.702 mmol, 1.4 equiv.) and Zn(OAc)2 (91.98 mg, 0.501 mmol, 1 equiv.) at room temperature. The resulting mixture was stirred for 16 h at 60 degrees C. The reaction was monitored by LCMS.The mixture was allowed to cool down to room temperature. The mixture was purified by reverse phase flash with the following conditions (Column:C18,330 g; Mobile Phase A: Water/0.05% NH4HCO3, Mobile Phase B:ACN; Flow rate:80 mL/min;Gradient: 35%B to 50%B in 15 min; Detector,220nm and 254nm) to afford crude product. The crude product (30 mg) was purified by Prep-HPLC with the following conditions (Column: XBridge Shield RP18 OBD Column, 5um,19*150mm; Mobile Phase A: Water(10MMOL/L NH4HCO3), Mobile Phase B: ACN; Flow rate: 25 mL/min; (1701) Gradient: 5% B to 16% B in 1 min; 254/220 nm; Rt: 7.47 min) to afford 4-chloro-5-[1-[(2- chloro-4-fluorophenyl)methyl]-1H,4H,5H,6H,7H-[1,2,3]triazolo[4,5-c]pyridin-5-yl]-2,3- dihydropyridazin-3-one(8.3mg,4.19%) as a white solid

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 15205-11-5.

Reference:
Patent; GOLDFINCH BIO, INC.; YU, Maolin; DANIELS, Matthew, H.; HARMANGE, Jean-christophe, P.; TIBBITTS, Thomas, T.; LEDEBOER, Mark, W.; WALSH, Liron; MUNDEL, Peter, H.; MALOJCIC, Goran; (860 pag.)WO2019/55966; (2019); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 1996-30-1, 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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

The title compound (150 mg, 12.7 %, off-white solid) was obtained from [4- [1- (5-] tributylstannanyl-isoxazol-3-yl)-ethyl]-piperazine-l-carboxylic acid ethyl ester (1.063 g, 1.98 mmol) and Pd (PPh3) [2C12] (19.2 mg) with [2-BROMO-4-CHLORO-1-FLUORO-BENZENE] (368mg, 1.76 mmol) in dioxane (lOmL) at 110 [C] overnight. 1H-NMR (CDC13) 8 (ppm): 7.94 (dd, 1H), 7.40 (m, 1H), 7.17 (dd, 1H), 6.71 (d, [1H),] 4.13 (q, 2H), 3.90 (q, 1H), 3.51 (m, 4H), 2.52 (m, 4H), 1.86 (d, 3H) and 1.26 (t, 3H).

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

Reference:
Patent; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2004/14370; (2004); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, 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 112-26-5, Application In Synthesis of 1,2-Bis(2-chloroethoxy)ethane

7.7Ig (50 mmo 1) of 2,6-dimethoxyphenol and 8.42 g (45 mmol) of 1,2- (dichloroethane) ethane were added to IOOml of acetonitrile at a temperature of 20 C with stirring , 6.06 g (108 mmol) of potassium hydroxide was added thereto, and the temperature was raised to 82 C. After 92 hours of reaction, acetonitrile was distilled off at atmospheric pressure to obtain orange turbid liquid.[0027] IOOml dichloromethane was added to the above-mentioned orange turbid liquid 1, the insoluble matter was filtered off, washed twice with 50 ml of IM sodium hydroxide solution and twice with saturated sodium chloride solution (20 C) Dried over anhydrous magnesium sulfate and evaporated to dryness at atmospheric pressure to give a yellow oily liquid 2;[0028] To the above yellow oily liquid 3 was added 25 ml of diethyl ether, the temperature was raised to 35 C, the insoluble matter was filtered off, cooled to _15 C, cooled for 3 hours, the liquid was stratified, and the pale yellow solution was taken and cooled to -15 C (2- (2,6-dimethoxyphenoxy) ethoxy) ethane in a yield of 69.33% and a purity of 98.42% as a white powder

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, 1,2-Bis(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Xi’an Modern Chemical Institute; Lu Tingting; Ji Yueping; Zhang Lijie; Liu Yajing; Wang Wei; Pan Yongfei; Xu Minghui; Mo Hongchang; Lu Xianming; Ding Feng; (6 pag.)CN106946664; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 64628-73-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 64628-73-5 name is 3-Chloro-4-(trifluoromethoxy)aniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A) 3-(3-Chloro-4-trifluoromethoxy-phenylamino)-propionic acid tert-butyl ester A solution of 9.26 g (42.4 mmol) of 3-chloro-4-trifluoromethoxy-phenylamine and 4.39 ml (42.4 mmol) of 2,6-lutidine in 50 ml of toluene was treated slowly with 7.30 ml (42.4 mmol) of tert-butyl 3-bromopropionate and stirred 2 days at reflux temperature. The reaction was then partitioned between aqueous 10% KHSO4 and EtOAc (3*). The organic phases were washed with 10% NaCl, dried over Na2SO4 evaporated and purified by flash silica gel column (n-heptane:EtOAc 9:1) to yield 9.59 g (60%) of the title compound as brown liquid. MS: 339 (M+, Cl).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-(trifluoromethoxy)aniline, and friends who are interested can also refer to it.

Reference:
Patent; Aebi, Johannes; Binggeli, Alfred; Green, Luke; Hartmann, Guido; Maerki, Hans P.; Mattei, Patrizio; US2011/92698; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 60811-21-4, 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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a dry-ice/ethanol cooled solution of compound S1 (20.0 g, 0.95 mol) in THF (200 mL) was added 2 M LDA (52 mL, 1.05 mol) dropwise over 30 min. After addition, the reaction mixture was stirred at this temperature for 30 min followed by the addition of DMF (10.5 g, 1.43 mol). The reaction was stirred for 30 min and warmed to room temperature slowly. The reaction mixture was then quenched with aq. NH4Cl (100 mL) and extracted with ethyl acetate (500 mL). The organic phase was washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated. The residue was purified by column chromatography on silica gel (eluted with petroleum ether/ethyl acetate=1:0 to 50:1) to give compound S2 (10 g, yield 40%) as a yellow oil.

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

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAK, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; (905 pag.)WO2017/35353; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics