HRID1276169

反应详情

EQUATION

反应方程式

HRID 1276169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,1'- Carbonyldiimidazole (13.6 g) was added to a solution of 2-amino-4-iodophenylamine (13.2 g) [see Makromol. Chem. (1993), 194(3), 859-868] in tetrahydrofuran (100 ml). The reaction mixture was stirred for 18 hours at room temperature, after which time the solvent was removed under reduced pressure, and the residue partitioned between 1N aqueous sodium hydroxide and diethyl ether. The aqueous was acidified with concentrated aqueous hydrochloric acid, and the resulting white precipitate filtered off and washed with water to afford 5-iodo-1,3-dihydro-2H-1,3-benzimidazol-2-one (14.0 g) as a white solid.

WORKUP

后处理

  1. customafter which time the solvent was removed under reduced pressure
  2. customthe residue partitioned between 1N aqueous sodium hydroxide and diethyl ether
  3. filtrationthe resulting white precipitate filtered off
  4. washwashed with water