Chlorides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, 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 61881-19-4, Product Details of 61881-19-4

To a solution of 28 (0.91 g, 1.7 mmol) in acetone (17 mL) wereadded CF3C(=NPh)Cl (0.53 mL, 3.3 mmol) and K2CO3 (1.1 g,8.3 mmol) at 0 C. After stirring for 2.5 h at the same temperature, thecompletion of the reaction was confirmed by TLC (5:1 n-hexane/EtOAc). The reaction mixture was filtered through Celite pad and thepad was washed with CHCl3. The filtrate and washings were concentrated.The resulting residue was purified by silica gel columnchromatography (25:1 n-hexane/EtOAc) to give 29 (1.2 g, quant.) ascolorless syrup. 1H NMR (500 MHz, CDCl3) delta 7.44-6.70 (m, 17H, Ar),5.08-4.83 (br m, 4H, H-1, H-2, H-3, H-4), 4.15-3.65 (br m, 3H, H-5, H-6a, H-6b), 1.08 (s, 9H, tBu), 1.01 (s, 9H, tBu); 13C NMR (125 MHz,CDCl3) delta 143.5, 143.3, 138.9, 138.6, 135.4, 135.3, 135.3, 135.2, 133.1,133.1, 128.7, 128.4, 128.4, 128.3, 128.2, 128.2, 128.1, 128.1, 128.0,127.9, 127.7, 127.7, 127.7, 126.9, 126.5, 126.2, 126.1, 126.1, 126.0,126.0, 125.6, 124.4, 119.4, 119.2, 84.0, 81.2, 80.0, 77.9, 77.7, 77.5,75.8, 75.5, 75.5, 73.9, 71.0, 68.8, 66.5, 66.2, 27.4, 27.0, 26.9, 22.7,20.0. HRMS (ESI) m/z: found [M+Na]+ 744.2935, C40H46F3NO6Sicalcd for [M+Na]+ 744.2939.

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Reference:
Article; Takato, Koichi; Kurita, Motoki; Yagami, Nahoko; Tanaka, Hide-Nori; Ando, Hiromune; Imamura, Akihiro; Ishida, Hideharu; Carbohydrate Research; vol. 483; (2019);,
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Application of 19752-55-7, 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

A 250 ml round-bottom flask was argonated and consecutively charged with Et2O (60 ml), Mg (1.31 g; 54.0 mmol), I2(one crystal), and a solution of 1-bromo-3,5-dichlorobenzene (12.54 g; 55.5 mmol) in Et2O (60 ml) was added in ca. 5 ml portions over 45 min. Stirring was continued for 3 h at RT, and a solution of 9c (9.52 g; 18.0 mmol) in hot toluene (60 ml, ca. 90 °C) was added slowly, and the mixture was heated to 40 °C for 15 h. A precipitate was decanted, washed with toluene (2 30 ml), treated with concd HClaq. (100 ml) at reflux for 3 h, and cooled to RT. The resulted precipitate was filtered, washedwith concd HClaq. (2 30 ml), and dried. Then, most of the beige solid was dissolved in a hot mixture of water (40 ml), concd HClaq. (120 ml) and ethanol (30 ml), resulted solution was decanted, cooled to RT, and part of the solvent (ca. 50 ml) wasslowly evaporated under reduced pressure. The resulted suspension was filtered, and collected filtrate was washed with concdHClaq. (2 30 ml), and dissolved in CH2Cl2 (150 ml). The organic phase was washed with brine (100 ml), and dried overMgSO4. Then, the mixture was filtered, n-heptane (40 ml) was added, and the mixture was slowly evaporated at 300 mbar (very slow rotations, no heating bath applied). The resulted precipitate was filtered, washed with n-hexane, and dried in vacuo. Filtrate was evaporated and the crystallization procedure was repeated. Both crops were collected and combined to obtain 10c (6.70 g; 9.07 mmol; 50percent calculated as a bromide) as a white solid.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-3,5-dichlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Grudzie?, Krzysztof; Basak, Tymoteusz; Barbasiewicz, Micha?; Wojciechowski, Tomasz M.; Fedory?ski, Micha?; Journal of Fluorine Chemistry; vol. 197; (2017); p. 106 – 110;,
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Adding a certain compound to certain chemical reactions, such as: 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine, 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 13078-79-0, Quality Control of 2-(3-Chlorophenyl)ethanamine

General procedure: 2.5mmol Thiazole-4-carboxyli acid and 2.0mmol amine were dissolved in 25mL DCM in a dry flask with continuous stirring, followed by the addition of 2.5mmol 3-(3-Dimethylaminopropyl)-1-Ethylcarbodiimide Hydrochloride (2.5mmol). When the temperature of the reaction system cooled to 0C, 50mg 4-dimethylaminopyridine (0.2mmol) was added dropwise and reacted for 1hat 0C. Then the reaction temperature was elevated to room temperature for another 4h. The reaction was stopped by adding 25mL saturated NaHCO3 solution and extracted twice with 20mL dichloromethane (2×20mL). The extracted organic layers were first dried by anhydrous Na2SO4, and then filtered and concentrated under vacuum distillation, obtaining the crude products. Finally, the crude products were further purified using column chromatography (ethy lacetate: petroleum ether, 1:5).

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:
Article; Li, Shengrong; Chen, Siyu; Fan, Jilin; Cao, Zhen; Ouyang, Weihao; Tong, Ning; Hu, Xin; Hu, Jie; Li, Peishan; Feng, Zifeng; Huang, Xi; Li, Yuying; Xie, Mingshan; He, Ruikun; Jian, Jingyi; Wu, Biyuan; Xu, Chen; Wu, Weijian; Guo, Jialiang; Lin, Jing; Sun, Pinghua; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 64 – 73;,
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Reference of 61881-19-4,Some common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, 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 the stirred suspension of p-methoxybenzyl alcohol (2.00 g, 14.5 mmol)and N-phenyl-2,2,2-trifluoroacetimidate chloride (3.40 g, 16.3 mmol) inDCM (70 mL), NaH (60% in mineral oil, 0.635 g, 15.8 mmol) was added portionwise at 0C.The mixture was stirred for 2h at rt. After an addition of ice, the organic phase was washedwith water (3 x 40 mL), dried (MgSO4), filtered, and evaporated. The resulting residue wascrystallized from Et2O/PE, to give 1 as white needles (4.00 g, 89%). mp 90-91C, 1H NMR(360 MHz in CDCl3, ppm): delta 7.37 (2H, br d, J = 8.5 Hz, Ph), 7.29 (2H, br t, J = 2.0 Hz, J =6.5 Hz, J = 7.5 Hz, Ph), 7.08 (1H, br t, J = 1.0 Hz, J = 7.0 Hz, J = 7.5 Hz, Ph), 6.92 (2H, br d,J = 8.5 Hz, Ph-OCH3, PMB), 6.82 (2H, br d, J = 8.5 Hz, Ph-OCH3, PMB), 5.25 (2H, s, CH2,PMB), 3.83 (3H, s, OCH3, PMB), 13C NMR (90 MHz in CDCl3, ppm): delta 160.08 (Cquat-OCH3,PMB), 145.28 (q, JC-C-F = 35,0 Hz), 144.58 (Cquat arom), 130.42, 128.89, 127.23, 124.04,119.73 (CH arom), 116.38 (q, JC-F = 285,5 Hz), 114.13 (Cm PMB), 69.69 (CH2,PMB), 53.32 (OCH3, PMB), HRMS (ESI) m/z [M+Na] 332.0869; found 332.0859, AnalCalcd C16H14F3NO2 : Calcd. C 62.13, H 4.56, N 4.53; found C 62.30, H 4.59, N 4.44.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, its application will become more common.

Reference:
Article; Barroca-Aubry, Nadine; Benchekroun, Mohamed; Gomes, Filipe; Bonnaffe, David; Tetrahedron Letters; vol. 54; 37; (2013); p. 5118 – 5121;,
Chloride – Wikipedia,
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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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C4H6Cl2

General procedure: In the initial mixed solution prepared in the round flask in Example 1, 3-chloro-2-(chloromethyl)prop-1-ene(50 [mu] L, 0.47 mmol)By following the same procedure as in Example 1 except for using 1-pyrene methanol (240 mg, 1.03 mmol)Experiments were conducted to obtain a solid state of the compound containing pyrene dimer, 120 mg in 49% yieldOctane-1,8-diol (99 mg, 0.68 mmol) (1 eq.)And 1-(bromomethyl)pyrene (440 mg, 1.49 mmol) (2.2 eq.),3 mL ([diol] = 50 mM) in anhydrous dimethylformamide in (DMF)To room temperature in the presence and condition of N2 and NaH (3 eq.), It was added to the round bottom flask. The mixed solution in the flask was stirred at room temperature for 1 hour.After that,Then quenched and diluted with distilled water was added to the solution.next, The organics were extracted by the addition of methyl-dichloro (DCM) to the mixed solution,The resulting organic layer was again distilled under reduced pressure to reotgo so that solution filtered through a filter containing sodium sulfate (Na2SO4).The resultant was purified by silica gel column chromatography (EtOAc: Hexane = 1: 5 (volume ratio)) of the solid state compound containing pyrene dimer increasing the purity of the resultant using,To give the 120 mg at a yield of 31%.

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 1871-57-4.

Reference:
Patent; Inha UniversityIndustry-AcademicCooperation Foundation; Jo, Dong Gyu; (29 pag.)KR101542140; (2015); B1;,
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Synthetic Route of 20850-43-5,Some common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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.

Under argon atmosphere, 17.5 ml of 1.58M n-butyl lithium-n-hexane solution was dropped into a mixture of 25 ml of tetrahydrofuran and 2.78 g of diisopropylamine under cooling ice, followed by 30 minutes’ stirring under the same condition. Thereafter a solution of 2.50 g of 1-tert-butoxycarbonyl-3-oxopiperazine (which was prepared by following Tetrahedron Lett., 1980, 21, 3019 – 3020) in 60 ml of tetrahydrofuran was added by dropping under cooling with ice, followed by 3 hours’ stirring under the same condition, further dropping of a solution of 2.30 g of 5-chloromethyl-benzo[1,3]dioxole in 20 ml of tetrahydrofuran under cooling with ice, and an hour’s stirring under the same condition. The solution was warmed to room temperature and stirred for 18 hours. After addition of saturated aqueous ammonium chloride solution, the solution was extracted with ethyl acetate, dried over anhydrous magnesium sulfate and the solvent was distilled therefrom under reduced pressure. The residue was purified on silica gel column chromatography (ethyl acetate) to provide 2.84 g (68%) of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonyl-3-oxopiperazine. 1H-NMR(CDCl3)delta:6.67(s,1H),6.65(d,J=1.3Hz,2H),5.90(s,2H), 4.52~4.43(m,1H),4.12(d,J=7.2Hz,2H),3.23(t,J=5.1Hz,2H), 2.57(t,J=5.8Hz,2H),1.45(s,9H) Mass,m/e:334(M+),278,144,57(base)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-(Chloromethyl)benzo[d][1,3]dioxole, its application will become more common.

Reference:
Patent; ASKA Pharmaceutical Co., Ltd.; EP1724267; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 2267-25-6, name is 2-Chloro-4-fluoroanisole, 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: 2-Chloro-4-fluoroanisole

To concentrated sulfuric acid (100mL) solution of2-chloro-4-fluoro anisole (38g, 237mmol), bromine (19mL, 737mmol) was addedunder ice-cooling, and the mixture was stirred for 1.5 hours. the reactionsolution was added gradually into ice water and extracted with diethyl ether(300mL × 3). After washing the organic layer with 5% aqueous sodium thiosulfatesolution (300 mL), the organic layer was dried over anhydrous magnesiumsulfate, filtered, and the crude product obtained through concentration underreduced pressure was purified by silica gel chromatography (hexane: ethylacetate = 1 : 0~10: 1) to give white solid of 5-bromo-2-chloro-4-fluoro anisole(8.0 g, yield: 14%) and white solid of 2-bromo-6-chloro-4- fluoro anisole (16.7g, yield: 30%).

The synthetic route of 2-Chloro-4-fluoroanisole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SAGAMI CHEMICAL RESEARCH INSTITUTE; KAKEN PHARMACEUTICAL COMPANY LIMITED; KOBAYASHI, OSAMU; TAKATSUNA, REIKO; NIIKURA, NAOKO; MATSUKAWA, TOMOKO; NAKAMURA, SHINJI; HIRAI, KENJI; KOCHI, SHINICHIRO; KAWANISHI, NAOKI; YAMADA, OSAMU; (75 pag.)JP2016/56157; (2016); A;,
Chloride – Wikipedia,
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Related Products of 7149-75-9, A common heterocyclic compound, 7149-75-9, name is 4-Chloro-3-methylaniline, molecular formula is C7H8ClN, 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.

Step 1 (0420) To a mixture of 4-chloro-3-methylphenylamine (350 mg), potassium carbonate (1.09 g) and N,N-dimethylformamide (10 mL) was added trifluoromethanesulfonic acid 2,2,2-trifluoroethyl ester (0.57 mL), and the mixture was stirred at an external temperature of 80° C. for 20 hours. The mixture was cooled to room temperature. After the mixture was diluted with ethyl acetate, and the resulting mixture was washed with water, saturated sodium hydrogen carbonate aqueous solution and brine successively, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: 0percent-10percent ethyl acetate:hexane, gradient elution) to give (4-chloro-3-methylphenyl)-(2,2,2-trifluoroethyl)amine (209 mg). (0421) 1H-NMR (CDCl3) delta ppm: 2.31 (3H, s), 3.65-3.90 (3H, m), 6.46 (1H, dd, J=8.5, 2.8 Hz), 6.55 (1H, d, J=2.8 Hz), 7.15 (1H, d, J=8.5 Hz).

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; Kissei Pharmaceutical Co., Ltd.; Inoue, Hitoshi; Ohno, Kohsuke; Nakamura, Tetsuya; Ohsawa, Yusuke; (58 pag.)US2016/362368; (2016); A1;,
Chloride – Wikipedia,
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Electric Literature of 38762-41-3, 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 38762-41-3 as follows.

f) Compound 1.7; A solution of 4-bromo-2-chloroaniline (4.00 g, 19.37 mmol), bis(pinacolato)diboron (5.90 g, 23.2 mmol) and KOAc (12.3 g, 58.1 mmol) in DMSO (100 mL) was deoxygenated by bubbling nitrogen through it for 45 min. PdCl2 (dppf) g, 1.94 mmol) and dppf (1.07 g, 1.94 mmol) were then added and the mixture was heated at 100C for 4 h. After cooling to room temperature the reaction mixture was diluted with EtOAc, washed successively with water and brine, dried (MgS04), filtered and concentrated under reduced pressure. The crude product was purified twice by flash chromatography using CH2Cl2 to give intermediate 1.7 (2.15 g, 44% yield) as a white solid.

According to the analysis of related databases, 38762-41-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GmbH; BOEHRINGER INGELHEIM PHARMA GmbH & CO KG; WO2005/118575; (2005); A1;,
Chloride – Wikipedia,
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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. 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

[4-(5-Chloro-6-fluoro-1H-benzoimidazol-2-yl)-phenyl]-methyl-(2-piperidin-1-yl-ethyl)-amine mp 167-168 C.

The synthetic route of 139512-70-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Millennium Pharmaceuticals, Inc.; US6348487; (2002); B1;,
Chloride – Wikipedia,
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