HRID1958772

反应详情

EQUATION

反应方程式

HRID 1958772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 3-(2-ethyl-4-formyl-6-methyl-phenyl)-acrylic acid methyl ester (5.93 g, 25.53 mmol) in MeOH (140 mL) and 2 N aq. NaOH (45 mL) was stirred at rt for 1 h. The MeOH was evaporated and the aq. solution was extracted twice with DCM. The aq. layer was acidified with 37% aq. HCl. The precipitate that formed was collected, washed with water and dried. The product was further purified by recrystallisation from EA (100 mL) to give 3-(2-ethyl-4-formyl-6-methyl-phenyl)-acrylic acid as yellow crystals (4.2 g). LC-MS: tR=0.87 min.

WORKUP

后处理

  1. customThe MeOH was evaporated
  2. extractionthe aq. solution was extracted twice with DCM
  3. customThe precipitate that formed
  4. customwas collected
  5. washwashed with water
  6. customdried
  7. customThe product was further purified by recrystallisation from EA (100 mL)