HRID1605076

反应详情

EQUATION

反应方程式

HRID 1605076 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3,4-dichlorophenyl)-1-hydroxy-3-methylurea (6 grams; 0.025 mol) in diethyl ether (200 ml), and triethylamine (4 ml) were charged into a glass reaction flask equipped with a mechanical stirrer. Phenyl chloroformate (4.2 grams; 0.027 mol) was added thereto. The reaction mixture was stirred, at room temperature, for a period of about one-half hour resulting in the formation of a precipitate. The precipitate was recovered by filtration, was washed with water, dried, and was recrystallized from a methylene chloride-pentane mixture to yield 1-(3,4-dichlorophenyl)-1-phenoxycarbonyloxy-3-methylurea melting at 93°C with decomposition and having the following elemental analysis as calculated for C15H12Cl2N2O4 :

WORKUP

后处理

  1. customequipped with a mechanical stirrer
  2. customresulting in the formation of a precipitate
  3. filtrationThe precipitate was recovered by filtration
  4. washwas washed with water
  5. customdried
  6. customwas recrystallized from a methylene chloride-pentane mixture