HRID1619081

反应详情

EQUATION

反应方程式

HRID 1619081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a suspension of 5-((E)-3-Dimethylamino-acryloyl)-1H-pyrrole-3-carboxylic acid ethyl ester (0.25 g, 1.06 mmol) in 4 mL of ethanol, guanidine hydrochloride (0.121 g, 1.27 mmol) and sodium ethylate (0.086 g, 1.27 mmol) were added. The mixture was heated to 110° C. overnight. Then, a further amount of sodium ethylate (0.086 g, 1.27 mmol) was added to the mixture and heating to 115° C. was prolonged for additional 24 hours. The resulting mixture was cooled at room temperature and diluted with water (2 mL). The solid was isolated by filtration, washed with 10 mL of water, dried in a vacuum oven at 40° C. affording to give 0.197 g (80%) of the title compound.

WORKUP

后处理

  1. additionwere added
  2. temperatureheating to 115° C.
  3. temperatureThe resulting mixture was cooled at room temperature
  4. customThe solid was isolated by filtration
  5. washwashed with 10 mL of water
  6. customdried in a vacuum oven at 40° C.
  7. customaffording