HRID2309181
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
CONDITIONS
反应条件
- 温度
- 5 °C
PROCEDURE
实验过程
To a solution of tert-butyl isocyanate (0.991 g) in methylene chloride (8 ml) was added dropwise to a mixture of N-amino-1,2,3,6-tetrahydropyridine hydrochloride (1.346 g) and triethylamine (1.012 g) in methylene chloride (40 ml) under ice bath cooling. The mixture was stirred for an hour at about 5° C. The reaction mixture was evaporated to dryness, and then the residue was dissolved in ethyl acetate (50 ml). The solution was washed with water (40 ml), dried over magnesium sulfate and evaporated to dryness. The crude residue was washed with ether and dried to give N-[(tert-butylcarbamoyl)amino]-1,2,3,6-tetrahydropyridine (0.50 g).
WORKUP
后处理
- temperaturecooling
- customThe reaction mixture was evaporated to dryness
- dissolutionthe residue was dissolved in ethyl acetate (50 ml)
- washThe solution was washed with water (40 ml)
- dry with materialdried over magnesium sulfate
- customevaporated to dryness
- washThe crude residue was washed with ether
- customdried