HRID1757535

反应详情

EQUATION

反应方程式

HRID 1757535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To thesolution placed in an ice bath was further added a solution of 1.94 g (10 mmol., purity 90.7%) of methyl 1-piperazinecarbodithioate in 4 ml of ethanol. The resulting mixture was then stirred for 30 min. at room temperature. To the mixture placed in an ice bath was dropwise added a solution of 2.12 g (10 mmol.) of propyl gallate in 4 ml of ethanol. The mixture was stirred overnight at room temperature and subsequently refluxed under heating for 4 hours. The mixture was cooled to room temperature. Precipitated crystals were collected by filtration and washedwith ethanol to give 1.848 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%.

WORKUP

后处理

  1. customTo thesolution placed in an ice bath
  2. customTo the mixture placed in an ice bath
  3. stirringThe mixture was stirred overnight at room temperature
  4. temperaturesubsequently refluxed
  5. temperatureunder heating for 4 hours
  6. temperatureThe mixture was cooled to room temperature
  7. customPrecipitated crystals
  8. filtrationwere collected by filtration and washedwith ethanol