HRID1170872

反应详情

EQUATION

反应方程式

HRID 1170872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-[butyl-(3-chloro-benzoyl)-amino]-5,6,7,8-tetrahydro-imidazo[1,2-a]pyridine-3-carboxylic acid ethyl ester (11.7 mmol) was dissolved in a solution of 190 mL MeOH/dioxan/4 M NaOH in water in a ratio of 15/4/1 and the solution was stirred over night at room temperature. The solvent was removed under vacuum, EtOAc (700 mL) was added thereto and the organic phase was washed with 0.5 M KHSO4 in water (700 mL). The aqueous phase was extracted with EtOAc (300 mL) and the combined organic phases were washed with saturated aqueous NaCl solution (700 mL) and dried over sodium sulphate, and the solvent was removed under vacuum. 4.13 g (94% over two stages) of the desired product 2-[butyl-(3-chloro-benzoyl)-amino]-5,6,7,8-tetrahydro-imidazo[1,2-a]pyridine-3-carboxylic acid were obtained.

WORKUP

后处理

  1. customThe solvent was removed under vacuum, EtOAc (700 mL)
  2. additionwas added
  3. washthe organic phase was washed with 0.5 M KHSO4 in water (700 mL)
  4. extractionThe aqueous phase was extracted with EtOAc (300 mL)
  5. washthe combined organic phases were washed with saturated aqueous NaCl solution (700 mL)
  6. dry with materialdried over sodium sulphate
  7. customthe solvent was removed under vacuum