HRID1811241

反应详情

EQUATION

反应方程式

HRID 1811241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of anhydrous sodium acetate (2.66 g, 82 mmol) in 140 ml of water was added with the solution of 5-tert-butoxycarbonylamino-3-oxo-pentanoic acid ethyl ester (4.20 g, 16.2 mmol) in 20 ml of absolute ethanol at room temperature. Upon completion of the addition, the mixture was stirred for 5 minutes, added with 2-amino-1-phenyl-ethanone (2.5 g, 14.6 mmol) and heated to reflux for 3 hours. The resulting mixture was added with water (300 ml), extracted with ethyl acetate (100 ml×3). The organic extracts were washed with brine (50 ml×3), dried with anhydrous sodium sulfate, filtered and concentrated to give 2-(2-tert-butoxycarbonylamino-ethyl)-4-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester (5.0 g, 88.7%).

WORKUP

后处理

  1. additionUpon completion of the addition
  2. temperatureheated
  3. temperatureto reflux for 3 hours
  4. extractionextracted with ethyl acetate (100 ml×3)
  5. washThe organic extracts were washed with brine (50 ml×3)
  6. dry with materialdried with anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated