HRID2225814

反应详情

EQUATION

反应方程式

HRID 2225814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-[2-Oxo-2-(1,2,3,4-tetrahydro-2-isoquinolinyl)ethoxy]-alpha-oxobenzeneacetic acid ethyl ester (0.3 g) in methanol (10 mL) was treated with sodium carbonate (0.113 g) in water (3 mL), and the mixture was stirred at room temperature for 20 minutes. After the solvents were removed in vacuo, water (10 mL) was added and the solution acidified with 3N hydrochloric acid, then the aqueous layer was extracted with dichloromethane-tetrahydrofuran (1:1). The organic layer was dried (MgSO4), evaporated and the residual solid was crystallized from acetone-tetrahydrofuran-hexane to yield 0.078 g of 4-[2-oxo-2-(1,2,3,4-tetrahydro-2-isoquinolinyl)ethoxy]-alpha-oxobenzeneacetic acid, mp 218°-220° C.

WORKUP

后处理

  1. customAfter the solvents were removed in vacuo, water (10 mL)
  2. additionwas added
  3. extractionthe aqueous layer was extracted with dichloromethane-tetrahydrofuran (1:1)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. customevaporated
  6. customthe residual solid was crystallized from acetone-tetrahydrofuran-hexane