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ChemicalBook CAS DataBase List 3-CHLORO-3-METHYL-1-BUTYNE
1111-97-3

3-CHLORO-3-METHYL-1-BUTYNE synthesis

4synthesis methods
-

Yield:1111-97-3 95%

Reaction Conditions:

with hydrogenchloride;sulfuric acid;zinc(II) chloride in water at 0 - 5; for 2 h;Reagent/catalyst;

Steps:

1.1 Step 1: Synthesis of 3-Chloro-3-methylbutyne
The process is shown in Figure 1. First, the chlorinated reactor is opened and returned to the freezing valve. The reaction vessel is cooled down to 10°C, and then hydrochloric acid, zinc chloride, and polyethylene glycol 600 are added in succession; -3 methyl butyne and sulfuric acid into the trough, pendingWhen the reactor temperature drops to 0°C, 3-hydroxy-3-methylbutyne and sulfuric acid are added dropwise to the reaction vessel. After the addition is completed, 0 to 5°C is maintained.The temperature of the reaction is 2 hours. After the reaction is completed, it is transferred to a washing kettle and washed. Then it is stirred and allowed to stand. The water layer is separated, and then it is transferred to the pumping kettle.Considering, suction filtration, and drying to give 3-chloro-3-methylbutyne (yield 95%, purity 99%);

References:

Jiangsu Lvye Agrochemical Co., Ltd.;Peng Ronggui;Chen Biao;Pei Jianhua;Yue Chengzhi CN107903181, 2018, A Location in patent:Paragraph 0007-0008; 0036-0040; 0054; 0058

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