HRID2361572

反应详情

EQUATION

反应方程式

HRID 2361572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of pyrrole ester 4b (8.2 g, 0.0392 mol), in ethanol and 100 mL of 10% potassium hydroxide were refluxed for 1 hour. The mixture was cooled and concentrated in vacuo to an oil. Water was added to the oil, the mixture acidified with dilute HCl and extracted with ether. The organic phase was dried with anh. sodium sulfate and concentrated in vacuo to a solid residue. The compound was recrystallized in 80 mL of ethanol to give 5.8 g of pure 3-acetyl-4,5-dimethyl-2-pyrrole carboxylic acid 5b as a solid. 1H NMR (DMSO-d6) δ 2.5 (s, 3H), 2.2 (s, 3H), 2.0 (s, 3H) ppm.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated in vacuo to an oil
  3. additionWater was added to the oil
  4. extractionextracted with ether
  5. dry with materialThe organic phase was dried with anh. sodium sulfate
  6. concentrationconcentrated in vacuo to a solid residue
  7. customThe compound was recrystallized in 80 mL of ethanol