HRID2270884

反应详情

EQUATION

反应方程式

HRID 2270884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

51 ml benzyloxycarbonyl chloride was dripped into a solution of 50 g (0.34 mole) DL-methionine amide in 200 ml water at 5-20° C., during which the pH was maintained at 7-9 with sodium hydroxide solution. A slimy precipitate formed immediately which became finely crystalline upon the addition of 200 ml MTBE. After the end of the addition the mixture was agitated 30 min further at room temperature. The precipitated, colorless crystals were then filtered off, washed with a little MTBE and recrystallized out of 700 ml toluene. After filtering off, washing with toluene and drying, 67 g (69%) Nαbenzyloxycarbonyl-DL-methionine amide with a melting point of 120-122° C. was obtained.

WORKUP

后处理

  1. customA slimy precipitate formed immediately which
  2. additionAfter the end of the addition the mixture
  3. filtrationThe precipitated, colorless crystals were then filtered off
  4. washwashed with a little MTBE
  5. customrecrystallized out of 700 ml toluene
  6. filtrationAfter filtering off
  7. washwashing with toluene
  8. customdrying