HRID461784

反应详情

EQUATION

反应方程式

HRID 461784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetylalanylalanylproline (2 mmole) and N-methylmorpholine (2 mmole) are dissolved in dry tetrahydrofuran (200 ml) and cooled to -20° to -25°. Isobutyl chloroformate (2 mmole) is added, and the mixture is stirred at -20° for 10 minutes. A solution of 2-azaalanyl-dl-lactamide (2 mmole) in tetrahydrofuran (10 ml) is added dropwise, and the mixture is allowed to warm to room temperature over a period of 2 hours and stirred for a further 3 hours. The precipitate is filtered off and the filtrate is evaporated to dryness. Chromatography of the residue on silica gel (70 gm) and elution with 18% methanol in chloroform gives acetylalanylalanylprolyl-2-azaalanyl-dl-lactamide.

WORKUP

后处理

  1. temperaturecooled to -20° to -25°
  2. stirringstirred for a further 3 hours
  3. filtrationThe precipitate is filtered off
  4. customthe filtrate is evaporated to dryness
  5. washChromatography of the residue on silica gel (70 gm) and elution with 18% methanol in chloroform