HRID2177681

反应详情

EQUATION

反应方程式

HRID 2177681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Lithium hydroxide monohydrate (0.075 g) was added to a solution of methyl 6-(benzenesulphonylmethyl)-2-ethyl-3-(furan-3-yl)benzoate (Intermediate 152, 0.092 g) in dioxane (1 ml) and water (1 ml) and the resultant solution was stirred and heated in the microwave at 150° C. for 4.5 hours. Ethyl acetate and water were added and the organic layer was separated, then acidified with concentrated hydrochloric acid. The mixture was extracted with ethyl aceate, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness then azeotroped with toluene. The residue was triturated with ether and the solid was collected by filtration and dried to give 6-(benzenesulphonylmethyl)-2-ethyl-3-(furan-3-yl)benzoic acid (0.027 g) as a white solid.

WORKUP

后处理

  1. customthe organic layer was separated
  2. extractionThe mixture was extracted with ethyl aceate
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness
  6. customthen azeotroped with toluene
  7. customThe residue was triturated with ether
  8. filtrationthe solid was collected by filtration
  9. customdried