HRID24540

反应详情

EQUATION

反应方程式

HRID 24540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 5-formyl-4-(2-ethoxycarbonylethyl)-3-methyl-1H-pyrrole-2-carboxylic acid ethyl ester (281 mg), 4-methyl-2-oxindole (147 mg) and piperidine (2 drops) in ethanol (2 mL) was stirred at 90° C. for 2 hours. Potassium hydroxide (213 mg) was added, the temperature was increased to 95° C. and held there for 1 hour. The reaction mixture was cooled and concentrated. The residue was dissolved into water and acidified with 2 N hydrochloric acid to pH 2. The precipitate was filtered, washed with water and dried in a vacuum oven overnight to give 337 mg (95%) of 4-(2-carboxyethyl)-3-methyl-5-(4-methyl-2-oxo-1,2-dihydroindol-3-ylidenemethyl)-1H-pyrrole-2-carboxylic acid.

WORKUP

后处理

  1. temperaturethe temperature was increased to 95° C.
  2. waitheld there for 1 hour
  3. temperatureThe reaction mixture was cooled
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved into water
  6. filtrationThe precipitate was filtered
  7. washwashed with water
  8. customdried in a vacuum oven overnight