反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To the solution 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 washed with ethanol to give 1.843 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%.
WORKUP
后处理
- customTo the solution placed in an ice bath
- customTo the mixture placed in an ice bath
- stirringThe mixture was stirred overnight at room temperature
- temperaturesubsequently refluxed
- temperatureunder heating for 4 hours
- temperatureThe mixture was cooled to room temperature
- customPrecipitated crystals
- filtrationwere collected by filtration
- washwashed with ethanol