反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of potassium hydroxide (4.9 g) in methanol (40 ml) was added 3-(4-isopropyl-1-piperazinyl)propylamine (14.7 g) and thereto was added carbon disulfide (6.0 g) under ice cooling over a period of 20 minutes. The resulting mixture was stirred for 3.5 hours under ice cooling. The reaction mixture was evaporated under reduced pressure. The residual oil was dissolved in water (40 ml) and washed with diethyl ether. The washed aqueous layer was ice-cooled and thereto was added methyl iodide (11.3 g) with stirring over a period of about 5 minutes. The resulting mixture was stirred for 2 hours under ice-cooling extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and then evaporated to give an oil of methyl N-[3-(4-isopropyl-1-piperazinyl)propyl]dithiocarbamate (15.6 g).
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- dissolutionThe residual oil was dissolved in water (40 ml)
- washwashed with diethyl ether
- temperaturecooled
- additionwas added methyl iodide (11.3 g)
- stirringwith stirring over a period of about 5 minutes
- stirringThe resulting mixture was stirred for 2 hours under ice-
- temperaturecooling
- extractionextracted with chloroform
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate
- customevaporated