HRID1576833

反应详情

EQUATION

反应方程式

HRID 1576833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring suspension of creatinine (11.88 g, 0.105 mole) in 100 ml dry DMF, p-chlorophenylisocyanate (15.36 g, 0.100 mole) is added dropwise with cooling. The mixture is stirred for 16 hours and then poured into about 500 ml of iced-water to yield the crystalline product which is filtered off, washed with water and recrystallized twice from acetone-methanol, once from tetrahydrofuran (THF) and then from DMF-methanol. The resultant pure 1-(1-methyl-4-oxo-2-imidazolidinylidene)-3-p-chlorophenylurea is dried in vacuo for 24 hours; m.p. 190°-2°C dec.

WORKUP

后处理

  1. additionis added dropwise
  2. temperaturewith cooling
  3. customto yield the crystalline product which
  4. filtrationis filtered off
  5. washwashed with water
  6. customrecrystallized twice from acetone-methanol, once from tetrahydrofuran (THF)
  7. dry with materialThe resultant pure 1-(1-methyl-4-oxo-2-imidazolidinylidene)-3-p-chlorophenylurea is dried in vacuo for 24 hours