HRID2165991

反应详情

EQUATION

反应方程式

HRID 2165991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzylmercaptan (24.8 g) was added dropwise to a solution of 10.8 of sodium methoxide in 100 ml ethanol. After stirring 15 minutes, the ethanolic solution of sodium benzylmercaptide was added dropwise to a solution of 30.8 g 2,4-dichlorothiazole [prepared by the method of P. Reynaud et al., Bull. Soc. Chim. France, 1735 (1962)], resulting in a temperature increase of 28° to 48°. When the exotherm subsided, the suspension was refluxed 1 hour, then the solvent was evaporated. Cold water (300 ml) was added to the oily residue, and the aqueous mixture was extracted with methylene chloride. The organic solution was washed with water, followed by saturated brine, then dried over magnesium sulfate, filtered and the solvent evaporated to give 43.8 g of 4-chloro-2-phenylmethylthiothiazole as a brown oil.

WORKUP

后处理

  1. customprepared by the method of P
  2. customFrance, 1735 (1962)], resulting in a temperature
  3. temperatureincrease of 28° to 48°
  4. temperaturethe suspension was refluxed 1 hour
  5. customthe solvent was evaporated
  6. additionCold water (300 ml) was added to the oily residue
  7. extractionthe aqueous mixture was extracted with methylene chloride
  8. washThe organic solution was washed with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. customthe solvent evaporated