HRID973736

反应详情

EQUATION

反应方程式

HRID 973736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.9 ml of triethylamine cooled to 0° to 5° C. were added to 10 g of mercapto-thiazoline in solution in 200 ml of methylene chloride, then 12 ml of benzyl chloroformate in solution in 60 ml of methylene chloride were added dropwise. After stirring for 3 hours at ambient temperature, the mixture was poured into an iced solution of N hydrochloric acid and the aqueous phase was extracted with methylene chloride. The organic phase was dried and concentrated to dryness and the residue was chromatographed on silica (eluant: hexane-ethyl acetate 7-3) to obtain 17.9 g of the expected product melting at 72° C.

WORKUP

后处理

  1. extractionthe aqueous phase was extracted with methylene chloride
  2. customThe organic phase was dried
  3. concentrationconcentrated to dryness
  4. customthe residue was chromatographed on silica (eluant: hexane-ethyl acetate 7-3)