HRID524977

反应详情

EQUATION

反应方程式

HRID 524977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

2.0 g (9.94 mmol) of 1-amino-N-phenyl-1H-pyrrole-2-carboxamide, 2.45 g (12.05 mmol) of (S)-2-(tert-butoxycarbonylamino)butanoic acid (purchased from Aldrich®, cat. no. 15533) and 1.90 g (12.24 mmol) of EDC.HCl were dissolved in a mixture of 90 mL of THF and 30 mL of dichloromethane. The resulting solution was heated at 55° C. overnight. Then the solvents were evaporated and the crude residue was taken up in dichloromethane and washed with an aqueous solution of sodium bicarbonate and brine. The organic layer was dried over magnesium sulphate, filtered and the solvent was evaporated. The solid obtained was triturated in diethyl ether to furnish 2.47 g (64% yield) of the title compound.

WORKUP

后处理

  1. customThen the solvents were evaporated
  2. washwashed with an aqueous solution of sodium bicarbonate and brine
  3. dry with materialThe organic layer was dried over magnesium sulphate
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customThe solid obtained
  7. customwas triturated in diethyl ether