2-Chloro-5-methylthiazole synthesis
- Product Name:2-Chloro-5-methylthiazole
- CAS Number:33342-65-3
- Molecular formula:C4H4ClNS
- Molecular Weight:133.6
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Yield: 93%
Reaction Conditions:
with t-butyl thionitrite;copper dichloride in acetonitrile at 25; for 2.66667 h;Inert atmosphere;
Steps:
1.1 (1) Preparation of 2-chloro-5-methylthiazole:
72 g (0.6 mol) of t-butyl sulfonitrile was dissolved in dry acetonitrile (1.5 L) to prepare a solution.The reactor was purged with nitrogen, then 65 g (0.48 mol) of dry anhydrous copper (II) chloride was added, and the prepared t-butyl sulfonitrile solution was added to the reaction vessel under vigorous stirring and nitrogen protection, and then kept. 2-Amino-5-methylthiazole (45.6 g, 0.40 mol) was added portionwise over a period of 40 min at 25 °C.The reaction mixture was reacted at 25 ° C for 2 h.Then 20% hydrochloric acid solution was added.The solvent was distilled off under reduced pressure, and then 300 ml of chloroform was added thereto, and 100 mL × 3 was washed with brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give 49.7 g of 2-chloro-5-methylthiazole, yield 93%;
References:
Zhejiang Yongtai Technology Co., Ltd.;Shao Hongming;Lin Jiaohua;Chen Shaoting;Li Yijun CN108164522, 2018, A Location in patent:Paragraph 0027; 0028; 0032; 0036
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