HRID388966

反应详情

EQUATION

反应方程式

HRID 388966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,4-diaminobenzoic acid (3 mmol) in DMF (10 mL) was charged with 1-isothiocyanato-2-trifluoromethylbenzene (3.3 mmol) and the resulting solution was stirred at RT for 4 h. After thiourea formation was complete, solid K2CO3 (10 mmol) was added to the reaction mixture, and the mixture was heated at 90° C. for 10 h. The reaction mixture was cooled to RT and acidified with 10% aqueous HCl to pH 7. The contents were poured onto ice cold water (30 mL) with vigorous stirring. The solid formed was collected by filtration, washed with water, and dried in vacuo to provide the product, 2-(2-trifluoromethylphenylamino)-1H-benzoimidazole-5-carboxylic acid as a yellow solid.

WORKUP

后处理

  1. temperaturethe mixture was heated at 90° C. for 10 h
  2. temperatureThe reaction mixture was cooled to RT
  3. additionThe contents were poured onto ice cold water (30 mL) with vigorous stirring
  4. customThe solid formed
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried in vacuo