HRID235544

反应详情

EQUATION

反应方程式

HRID 235544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.95 g (25.7 mmol) of 2-chloro-4-trifluoromethyl-5-thiazolecarbonyl chloride in 50 ml of anhydrous ether was added dropwise at 0° C. to a mechanically stirred mixture of ethyl mercaptan (2.1 ml, 28.3 mmol) and triethylamine (3 g, 30 mmol) in 100 ml of anhydrous ether. The workup for this reaction was the same as Example 1 except that the crude pale yellow oil was distilled in a Kugelrohr at 80° C./0.55 mm to yield a colorless oil, 5.59 g. This oil was crystallized from petroleum ether at -72° C. to yield ethyl 2-chloro-4-trifluoromethyl-5-thiazolecarbothioate as a white solid; 4.8 g (68% yield), mp 28°-32° C.

WORKUP

后处理

  1. distillationwas distilled in a Kugelrohr at 80° C./0.55 mm
  2. customto yield a colorless oil, 5.59 g
  3. customThis oil was crystallized from petroleum ether at -72° C.