HRID2111876

反应详情

EQUATION

反应方程式

HRID 2111876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5[4-(4-(2-amino-2-methoxycarbonylethyl)phenoxy)benzylidene]thiazolidin-2,4-dione hydrochloride (2.5 g, 5.76 mmol) and N-Boc-pyrolidin-2-carboxylic acid (1.238 g, 5.76 mmol) in dimethyl formamide (25 ml) was stirred for 60 minutes at 0° C. N,N′-Dicyclohexylcarbodiimide (1.423 g, 6.91 mmol) was added to it and stirring was continued for 10 h at ambient temperature. Water (200 ml) was added to the reaction mixture and stirred for 15 minutes. Ethyl acetate (200 ml) was added to the reaction mixture and stirring continued for another 15 minutes. The organic layer was separated, washed with water (75 ml), dried over anhydrous sodium sulphate and concentrated to afford the crude product, which was purified by column chromatography to furnish the required product (1.1 g, yield 32.4%).

WORKUP

后处理

  1. stirringstirred for 15 minutes
  2. stirringstirring
  3. waitcontinued for another 15 minutes
  4. customThe organic layer was separated
  5. washwashed with water (75 ml)
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationconcentrated
  8. customto afford the crude product, which
  9. customwas purified by column chromatography