HRID1415638

反应详情

EQUATION

反应方程式

HRID 1415638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of N-(2-aminophenyl)-2-dimethylaminoacetamide (8.9 g) (prepared as described in Example 6) in acetonitrile (50 ml) was treated with ethoxycarbonyl isothiocyanate (6.4 g), dropwise with stirring, maintaining the temperature at 15°-20° C. by external cooling. When the addition was complete, the solid had dissolved but after being left to stand for a further 5 minutes, another solid precipitated. This was filtered off and washed with ice-cold acetonitrile to give 1-ethoxycarbonyl-3-(2-dimethylaminoacetamidophenyl)thiourea (9.4 g), m.p. 159°-160° C. (with decomposition).

WORKUP

后处理

  1. temperaturemaintaining the temperature at 15°-20° C. by external cooling
  2. additionWhen the addition
  3. dissolutionthe solid had dissolved
  4. waitafter being left
  5. customanother solid precipitated
  6. filtrationThis was filtered off
  7. washwashed with ice-cold acetonitrile