HRID24537

反应详情

EQUATION

反应方程式

HRID 24537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

4-(2-carboxyethyl)-3-methyl-5-(5-chloro-2-oxo-1,2-dihydroindol-3-ylidenemethyl)-1H-pyrrole-2-carboxylic acid suspended in ethylene glycol (5 mL) was heated in a sealed tube in a pre-heated oil bath at 200° C. for 2 hours. The reaction mixture was cooled to 90° C. and potassium hydroxide (2 pellets) were added. The mixture was then heated at 90° C. for 30 minutes, after which time it was cooled, poured into water, and acidified with 2 N hydrochloric acid to pH 2. The precipitate that formed was filtered, washed with water, and dried in a vacuum oven overnight to give 77 mg (29%) of 3-[2-(5-Chloro-2-oxo-1,2-dihydroindol-3-ylidenemethyl)-4-methyl-1H-pyrrol-3-yl]-propionic acid.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 90° C.
  2. temperatureThe mixture was then heated at 90° C. for 30 minutes
  3. temperatureafter which time it was cooled
  4. customThe precipitate that formed
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried in a vacuum oven overnight