HRID24533

反应详情

EQUATION

反应方程式

HRID 24533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

5-Formyl-4-(2-methoxycarbonylethyl)-3-methyl-1H-pyrrole-2-carboxylic acid ethyl ester (80.2 g), 2-oxindole (37.9 g) and ethanol (300 mL) were warmed to 70° C. in a 500 mL, 3-neck round bottom flask equipped with mechanical stirring and a reflux condenser. Piperidine (1.3 g) was added and the mixture was refluxed for 4 hours. The mixture was cooled to 10° C. and the orange precipitate collected by vacuum filtration and washed with 30 mL of ethanol. The solid was slurry-washed in 150 mL of refluxing ethanol, cooled, collected by vacuum filtration, washed with 30 mL of ethanol and vacuum dried to give 81.7 g (75%) of 4-(2-Methoxycarbonylethyl)-3-methyl-5-(2-oxo-1,2-dihydroindol-3-ylidenemethyl)-1H-pyrrole-2-carboxylic acid ethyl ester as an orange solid.

WORKUP

后处理

  1. customequipped
  2. temperaturethe mixture was refluxed for 4 hours
  3. filtrationthe orange precipitate collected by vacuum filtration
  4. washwashed with 30 mL of ethanol
  5. washThe solid was slurry-washed in 150 mL of refluxing ethanol
  6. temperaturecooled
  7. filtrationcollected by vacuum filtration
  8. washwashed with 30 mL of ethanol and vacuum
  9. customdried