HRID630689
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 a 100 mL three-neck flask, 10.0 g (56.4 mmol) of 2-oxo-2-phenylethyl thiocyanate and 3.73 g (56.4 mmol) of malononitrile were dissolved in 60 mL of ethanol and admixed with 5.14. g (50.8 mmol) of triethylamine in a gradual manner, so the temperature did not climb above 30° C. This was followed by stirring at room temperature for 12 h. The reaction mixture was diluted with 50 mL of water and acidified with glacial acetic acid. The precipitated solid was separated off and washed three times with 10 mL of a 10:10:1 mixture of water:ethanol:glacial acetic acid each time. The solid was dried to obtain 11.1 g (49.1 mmol) of (4-phenyl-1,3-thiazol-2-yl)malononitrile.
WORKUP
后处理
- customdid not climb above 30° C
- customThe precipitated solid was separated off
- washwashed three times
- additionwith 10 mL of a 10:10:1 mixture of water
- customThe solid was dried