HRID1475746

反应详情

EQUATION

反应方程式

HRID 1475746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4.5 g of 7-(2-m-tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic acid 2-m-tolyl-ethyl ester and 650 mg of sodium hydroxide were dissolved in 50 ml of methanol, 50 ml of THF and 5 ml of water. The mixture was kept at room temperature for 20 h, then stirred at 50° C. for 5 h and evaporated. The residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide and washed three times with 50 ml each of diisopropyl ether. The pH was adjusted to 2 with sodium hydrogensulfate and the mixture stirred for 30 min at room temperature. The product was collected by filtration, washed and dried in vacuo to yield 3.1 g of the title compound.

WORKUP

后处理

  1. customevaporated
  2. dissolutionThe residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide
  3. washwashed three times with 50 ml each of diisopropyl ether
  4. stirringthe mixture stirred for 30 min at room temperature
  5. filtrationThe product was collected by filtration
  6. washwashed
  7. customdried in vacuo