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ChemicalBook CAS DataBase List 3-Chloro-2-butanone

3-Chloro-2-butanone synthesis

10synthesis methods
-

Yield:4091-39-8 12.6%

Reaction Conditions:

with hydrogenchloride;dihydrogen peroxide;copper dichloride at 35 - 78; for 5.25 h;

Steps:

7
equipped with a stirrer, a condenser and a constant pressure funnel 250 ml three-necked flask, 43.27 g, 0.6 moles XVI-butanone and 36% HC1 30. 42 g, 0.3 mol, Cupric chloride 8.1 g, 0.06 mol, 35 degrees Celsius, was slowly added dropwise 30% H202 49. 23 Ke 15 minutes, 0.39 mole, after completion, the reaction was heated to reflux for 5 hours 78 ° C, the reaction mixture was cooled to room temperature, the organic phase was separated, washed with saturated sodium carbonate solution twice, dried over anhydrous sodium sulfate, distillation to collect 137-140 ° C fraction, to give a brown liquid chloroprene 3- one XVII8. 0 g, yield rate of 12.6%; after 100 ml round bottom flask, and 30 ml of ethanol was added thiourea 3.5 g, 47 mmol, thiourea was stirred heated under reflux until dissolved, 5.0 g, 47 mmol 3- chloroprene ketone XVII, after refluxing overnight, concentrated to remove the ethanol yield a crude yellow solid, dissolved in 30 ml of dichloromethane, washed with saturated sodium carbonate solution, the organic layer was collected, dried over anhydrous sodium sulfate, and concentrated to give a yellow oil mixed with a solid substance 2 - amino-3,4-dimethyl-thiazol XVII13 8 g, yield 63.3%.

References:

Jiangxi Tianren Ecology Co., Ltd.;Nankai University;Chen, Xiaoyan;Liu, Xiping;Fan, Zhijin;Liang, Xiaowen;Li, Yuedong;Mao, Wutao;Li, Juanjuan;Wang, Dun;Wang, Shuhua;Zhou, Lifeng;Ji, Xiaotian;HUA, XUEWEN CN102942565, 2016, B Location in patent:Paragraph 0042-0043; 0093-0094

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