HRID263267

反应详情

EQUATION

反应方程式

HRID 263267 的结构方程式

PROCEDURE

实验过程

In a nitrogen atmosphere, 24.8 g. (0.3 mole) 2-methyl-2-aminopropionitrile and 30.7 g. (0.3 mole) t-butyl isocyanate, 97%, are combined and stirred for 5 minutes. At the end of this period, the mixture is filtered and 1 ml. of pyridine is added to the filtrate. This mixture is heated in an oil bath for one and one-half hours, keeping the temperature of the bath below 70°. The solid is recrystallized from methanol:water, 60:40, to give N-(1-cyano-1-methylethyl)-N'-(1,1-dimethylethyl)urea, m.p. 204°-5°; Anal. Calcd. for C9H17N3O; C: 58.99, H: 9.35, N: 22.93; Found: C: 59.21, H: 9.26, N: 22.59.

WORKUP

后处理

  1. filtrationAt the end of this period, the mixture is filtered
  2. additionof pyridine is added to the filtrate
  3. temperatureThis mixture is heated in an oil bath for one and one-half hours
  4. customthe temperature of the bath below 70°
  5. customThe solid is recrystallized from methanol