HRID1283825

反应详情

EQUATION

反应方程式

HRID 1283825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While cooling and stirring 250 g. of pyridine, 175 g. (1.40 moles) of thiazolidine hydrochloride [preparation described by S. Ratner and H. Clarke, J. Am. Chem. Soc. 59, 200 (1937)] was added. After it had dissolved, 106.4 g. (1.40 mole) of carbon disulfide was added dropwise, followed by 128.5 g. (0.70 mole) of anhydrous zinc acetate. The resulting reaction mixture was stirred at 40° - 50°C for 2 hours. The precipitate was filtered at 5° - 10°C. The crude solid was water-washed and finally freed of pyridine by vacuum-drying at 120°C. to give 147.8 g. of the desired product. It gradually decomposed starting at ca. 200°C without a definite final decomposition point. A small sample washed with hot benzene had the following analysis:

WORKUP

后处理

  1. temperatureWhile cooling
  2. dissolutionAfter it had dissolved
  3. customThe resulting reaction mixture
  4. stirringwas stirred at 40° - 50°C for 2 hours
  5. filtrationThe precipitate was filtered at 5° - 10°C
  6. washwashed
  7. customby vacuum-drying at 120°C.
  8. customto give 147.8 g