Category: chlorides-buliding-blocks

2770-11-8, name is 2-(4-Chlorophenoxy)aniline, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 2770-11-8

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.

The synthetic route of 2770-11-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Weidner, Thomas; Nasereddin, Abed; Preu, Lutz; Gruenefeld, Johann; Dzikowski, Ron; Kunick, Conrad; Molecules; vol. 21; 2; (2016);,
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Electric Literature of 61881-19-4, 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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3,4,6-Tri-O-benzyl-2-deoxy-2-trichloroacetamido-alpha/beta-D-galactopyranosyl N-phenyltrifluoroacetimidate (181). The hemiacetal (1.85 g, 3.11 mmol), obtained from the thioglycoside 24, was dissolved in acetone (31 mL). N-(phenyl)trifluoroacetimidoyl chloride (1.29 g, 6.22 mmol) and Cs2CO3 (1.12 g, 3.42 mmol, 1.1 equiv.) were added to the solution. The mixture was stirred for 4 h at rt. The reaction mixture was filtered and concentrated. The residue was purified by flash chromatography (Chex/EtOAc 85:15 to 7:3 + 1% Et3N) to give N-phenyltrifluoroacetimidate 181 (2.10 g, 88%) as a light yellow oil. 1H NMR (CDCl3), delta 7.61-7.09 (m, 18H, HAr), 6.77 (d, 2H, J = 7.6 Hz, HAr), 6.48 (do, 1H, JNH,2 = 7.7 Hz, NH), 6.47 (bso, 1H, H-1), 4.97 (d, 1H, J = 11.4 Hz, HBn), 4.76 (dpo, 1H, J = 11.9 Hz, HBn), 4.73 (m, 1H, H-2), 4.64 (d, 1H, HBn), 4.57-4.48 (m, 3H, HBn), 4.20 (bs, 1H, H-4), 4.07 (pt, 1H, H-5), 3.88 (dd, 1H, J2,3 = 11.0 Hz, J3,4 = 1.4 Hz, H-3), 3.72 (pt, 1H, J5,6a = 7.8 Hz, H-6a), 3.62 (dd, 1H, J5,6b = 5.7 Hz, J6a,6b = 9.1 Hz, H-6b). 13C NMR (CDCl3), delta 161.8 (NHCO), 143.1, 138.0, 137.7, 137.0 (4C, CIVAr), 129.4-119.3 (20C, CAr), 94.3 (C-1, 1JCH = 162.9 Hz), 92.3 (CCl3), 75.5 (C-3), 74.8, 73.7 (2C, CBn), 72.5 (C-5), 71.6 (C-4), 71.3 (CBn), 68.1 (C-6), 50.6 (C-2).

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, 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; INSTITUT PASTEUR; Centre National de la Recherche Scientifique; Institut National De La Sante Et De La Recherche Medicale; UNIVERSITE PARIS DESCARTES; Mulard, Laurence; Chassagne, Pierre; Sansonetti, Philippe; EP2724730; (2014); A1;,
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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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., SDS of cas: 19752-55-7

3,5-dichlorobromobenzene (2.3 g, 10 mmol), 9-phenylcarbazole-3-boronic acid (2.5 g, 11 mmol) Sodium carbonate (5.1 g, 48 mmol), Pd2 (dba) 3 (0.4 g, 0.4 mmo 1), Toluene, ethanol, water 50ml in turn added to the reaction bottle, The reaction was refluxed under nitrogen for 10 hours, Cooled to room temperature, separated, and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with saturated brine and water respectively. The organic layer was dried over magnesium sulfate, filtered, The column was silica gel to give 3.0 g of product, HPLC purity 99.2percent.

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Li Chong; Yu Kaichao; Zhang Zhaochao; (42 pag.)CN107098918; (2017); A;,
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20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C8H7ClO2

General procedure: Suspension of the appropriate 3-amino-1,1-dioxo-1,4,2-benzodithiazine derivative 4a-h (0.5 mmol), anhydrous K2CO3 (1.5 mmol, 0.21 g) and the appropriate alkyl chloride (0.6 mmol) in dry THF (5 ml) was heated at reflux for 20-24 h, then cooled in ice-bath and filtered off. The crude product was suspended in 5 ml of water, heated gently to ca. 50 C; and cooled with vigorous stirring until granular precipitate appeared. Filtering off and washing with cold water and diluted EtOH gave pure potassium salts. 4.5.7 ;N-{2-[(1,3-Benzodioxol-5-yl)methylthio]-4-chloro-5-(5-phenyl-1,3,4-thiadiazol-2-yl)benzenesulfonyl}cyanamide potassium salt (5k) ;Starting from 4c (0.204 g) and 1,3-benzodioxol-5-ylmethyl chloride (0.102 g). Yield: 0.287 g (99%): m.p. 285-287 C; IR (KBr): nu 3443, 2924, 2853, 2179, 1652, 1623, 1577, 1501, 1489, 1357, 1129 cm-1; 1H NMR (500 MHz, DMSO-d6): delta 4.35 (s, 2H, SCH2), 6.01 (s, 2H, OCH2O), 6.89 (d, J = 7.81 Hz, 1H, Ar), 6.97 (d, J = 7.81 Hz, 1H, Ar), 7.05 (s, 1H, Ar), 7.58-7.60 (m, 3H, Ar), 7.68 (s, 1H, Ar), 8.07-8.08 (m, 2H, Ar), 8.69 (s, 1H, Ar); Anal. C23H14ClKN4O4S3 (C, H, N).

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Brozewicz, Kamil; Slawinski, Jaroslaw; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 384 – 394;,
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Reference of 106-39-8,Some common heterocyclic compound, 106-39-8, name is 1-Bromo-4-chlorobenzene, molecular formula is C6H4BrCl, 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: In a thermostatted bath at 25C (or 60C for compounds 18 and 28), a 25 mL Schlenk flask was charged in air with a magnetic stir bar, arylbromide (0.5 mmol), arylboronic acid (0.6 mmol), K2CO3 (0.6 mmol), 1 (26.6 mg, 1mol-%), ethanol (1.5 mL), and water (0.5 mL). The reaction mixture was kept under vigorous stirring until the GC control showed no residual aryl bromide in solution. Water (10 mL) was added to the suspension and the organics were extracted with dichloromethane (3×10 mL). The solution was dried over Na2SO4 and then passed through a column filled with silica gel (diatomaceous earths were used in the case of compound 28). Elimination of the solvent under vacuum gave the desired biaryl as white microcrystalline solid. Purity (96÷99%) was established by GC and 1H NMR. 1H and 13C{1H} NMR data of compounds 8-28. Spin multiplicity is given by s=singlet, br s=broad singlet, q=quartet, st=septet, qq=quartet of quartets, ddd=doublet of doublets of doublets, m=unresolved multiplet. 4-Chloro-4′-methyl-1,1′-biphenyl (16). Yield 96%. C13H11Cl (202.68): calcd. C 77.04, H 5.47; found C 76.95, H 5.48. 1H NMR (CDCl3): delta = 7.55-7.33 (6H, m), 7.29-7.16 (2H, m), 2.39 (3H, s, CH3) ppm. 13C NMR (CDCl3): delta = 139.5, 137.4, 137.0, 132.9, 129.5, 128.8, 128.1, 126.7, 21.0 (CH3) ppm.

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-4-chlorobenzene, its application will become more common.

Reference:
Article; Del Zotto, Alessandro; Colussi, Sara; Trovarelli, Alessandro; Inorganica Chimica Acta; vol. 470; (2018); p. 275 – 283;,
Chloride – Wikipedia,
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Related Products of 1005-56-7,Some common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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 solution of cholesterol (863 mg, 2.23 mmol) in CH2Cl2 (10 mL) were added pyridine (485 muL, 6.00 mmol) and phenyl chlorothionoformate (277 muL, 2.00 mmol) (For other substrates, CH3CN was used in place of CH2Cl2.). The mixture was stirred at room temperature for 50 min and diluted with EtOAc. The solution was washed with brine and dried over anhydrous MgSO4. After concentration, the residue was purified by flash chromatography on silica gel (hexane?hexane/EtOAc=10/1) to give thiocarbonate 5b (1.04 g, 1.99 mmol, 100%).

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

Reference:
Article; Kobayashi, Shoji; Kuroda, Hiroyuki; Ohtsuka, Yuta; Kashihara, Takashi; Masuyama, Araki; Watanabe, Kiyoshi; Tetrahedron; vol. 69; 10; (2013); p. 2251 – 2259;,
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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. 623-12-1, name is 1-Chloro-4-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Chloro-4-methoxybenzene

General procedure: Palladacycle C1 (0.005mmol), olefin (0.75mmol), aryl chloride (0.5mmol), K2CO3 (1.0mmol) and DMF/H2O (2ml, 1:1) were added to a small tube and the mixture was heated to 110C for 6h in the presence of air. The reactions were monitored by thin-layer chromatography (TLC). At the end of the cross-coupling reactions, the mixture was cooled, extracted with n-hexane:EtOAc (8:2), filtered and purified by recrystallization from ethanol and water or purified by silica gel column chromatography (n-hexane:EtOAc, 8:2).

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; Javad Sabounchei, Seyyed; Hashemi, Ali; Yousefi, Abed; Gohari Derakhshandeh, Parviz; Karamian, Roya; Asadbegy, Mostafa; Van Hecke, Kristof; Polyhedron; vol. 135; (2017); p. 1 – 9;,
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Application of 886762-39-6, These common heterocyclic compound, 886762-39-6, name is 3,4-Dichloro-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.

Example 31 (£)-N-(4-((3,4-Dichloro-2-fluorophenyl)a^ 2H-[l,4]dioxino[2,3-c]pyrrol-6(3 -yl)but-2-enamide Step 1) N-(3,4-dichloro-2-fluorophenyl)-7-fluoro-6-nitroquinazolin-4-amine A solution of 4-chloro-7-fluoro-6-nitroquinazoline (10.00 g, 44.0 mmol) and 3,4-dichloro-2-fluoroaniline (8.40 g, 46.5 mmol) in isopropanol (150 mL) was heated to 70 C and stirred for 5.0 hours. The reaction mixture was then cooled to 25 C, and a yellow solid precipitated out. The mixture was filtered. The filtered cake was washed with isopropanol (50 mL) and dried under vacuum to give the title compound as a yellow solid (11.4 g, 70.0%). The compound was characterized by the following spectroscopic data: MS (ESI, pos.ion) m/z : 371.0 [M+H]+.

The synthetic route of 886762-39-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; LIU, Bing; LIU, Jinlei; ZHANG, Jiancun; ZHENG, Changchun; WO2014/177038; (2014); 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. 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

Taking 0.01 muM structure 1 and 0.04 muM structure 3 by adding three-mouth flask, nitrogen protection, magnetic stirring dissolved in 200 ml dichloromethane in, ice water bath. In the slowly dripping triethylamine in three mouth bottle, during the dropping will be accompanied by white mist generating, heating up to 40 C, this temperature is kept continuous stirring 8 hours. The reaction liquid washing three times with saturated sodium chloride solution, adding anhydrous magnesium sulfate standing drying, after clarifying filtration, vacuum hangs steams to remove the solvent, to obtain orange crystal that aromatic module including cup and cyclic phosphate ester flame retardants, yield 85.39%.

The synthetic route of 4090-55-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese People’s Armed Police Force Academy; Lu Lingang; Wang Huiya; Qian Xiaodong; Yang Shousheng; Jin Jing; (8 pag.)CN107778328; (2018); A;,
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Reference of 1871-57-4,Some common heterocyclic compound, 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, molecular formula is C4H6Cl2, 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 1; Example 1 -1; 5.3 g of methallyl dichloride and 11.9 g of tri(ethylene glycol)monomethyl ether) were put into a reactor, and then 60 mL of tetrahydrofuran was added thereto. To the mixture was added dropwise 3.84 g of sodium hydride. The reactor was kept at 65 0C for 12 hr. 5 mL of water was added dropwise to the reactor. The reaction mixture was evaporated under vacuum to remove the tetrahydrofuran. The concentrate was extracted with 100 mL of diethyl ether and 100 mL of water. The organic layer was subjected to column chromatography using ethyl acetate/methanol (100/0-80/20), giving the compound of Formula 12 in a yield of 35%. 1H NMR (250 MHz, CDCl3): delta 5.18 (s, 2H; CH2), 4.01 (s, 4H; CH2(CH2O)2), 3.70-3.58 (m, 24H; OCH2), 3.37 (s, 6H; OCH3)

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

Reference:
Patent; INDUSTRY-ACADEMIC COOPERATION FOUNDATION, YONSEI UNIVERSITY; JANG, Woo-Dong; CHOI, Kwang-Mo; WO2010/93128; (2010); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics