HRID1828196

反应详情

EQUATION

反应方程式

HRID 1828196 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

1,3-Dimethyl-5-(2-nitro-propenyl)-1,3-dihydro-benzoimidazol-2-one (2.23 g) was dissolved in methanol (15 mL) and water (40 mL) and treated sequentially with iron (1.67 g) and iron trichloride hexahydrate (174.3 mg). After heating to 75° C. concentrated hydrochloric acid (8 mL) was added in portions over 0.5 hours. The mixture was stirred at 75° C. for 2.5 hours, cooled, treated with saturated sodium bicarbonate and extracted into ethyl acetate The organic layer was dried over sodium sulfate, and concentrated to give 1,3-Dimethyl-5-(2-oxo-propyl)-1,3-dihydro-benzoimidazol-2-one (1.465 g).

WORKUP

后处理

  1. additionwas added in portions over 0.5 hours
  2. temperaturecooled
  3. extractionextracted into ethyl acetate The organic layer
  4. dry with materialwas dried over sodium sulfate
  5. concentrationconcentrated