HRID1248744

反应详情

EQUATION

反应方程式

HRID 1248744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 300 ml of tetrahydrofuran were dissolved 40.0 g of N-t-butoxycarbonyl-leucyl-glycine and 38.8 g of pentachlorophenol, after which 30.0 g of dicyclohexylcarbodiimide (DCC) was added with ice-cooling, and the resulting mixture was subjected to reaction overnight. The insoluble material was collected by filtration and the solvent was removed by distillation to obtain a solid, which was recrystallized from ethyl acetate and petroleum ether to obtain N-t-butoxycarbonyl-leucyl-glycine-pentachlorophenyl ester. Yield: 65.9 g (88.5%). [α]D24 =-23.4° (C=1, dimethylformamide). Melting point (Mp): 155°-157° C.

WORKUP

后处理

  1. temperaturecooling
  2. customthe resulting mixture was subjected to reaction overnight
  3. filtrationThe insoluble material was collected by filtration
  4. customthe solvent was removed by distillation
  5. customto obtain a solid, which
  6. customwas recrystallized from ethyl acetate and petroleum ether