HRID1291225
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was further refluxed for 13 hours
- temperatureThe mixture was cooled to room temperature
- filtrationthe resulting precipitate was collected by filtration
- washwashed with ethanol and ether
- customdried under reduced pressure