HRID1291225

反应详情

EQUATION

反应方程式

HRID 1291225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methylhydrazine (1.82 g) and 3-ethoxycarbonyl-4,5-dimethyl-2-formylpyrrole (3.85 g) in ethanol (40 ml) was refluxed for 2 hours. After cooling to room temperature, concentrated sulfuric acid (0.7 ml) was added and the mixture was further refluxed for 13 hours. The mixture was cooled to room temperature and the resulting precipitate was collected by filtration, washed with ethanol and ether, and dried under reduced pressure to provide the title compound as light-yellow powder (3.64 g; yield 100%). 1H-NMR (DMSO-d6) δ: 2.26(6H,s), 3.62(3H,s), 7.98(1H,s), 11.6-11.7(1H,m).

WORKUP

后处理

  1. temperaturethe mixture was further refluxed for 13 hours
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationthe resulting precipitate was collected by filtration
  4. washwashed with ethanol and ether
  5. customdried under reduced pressure