HRID47044

反应详情

EQUATION

反应方程式

HRID 47044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 g (0.0033 mol) of L-alanyl-L-proline ethylamide hydrobromide was dissolved in 20 ml of dry pyridine and 0.45 ml of pivaloyl chloride was added. The mixture was stirred for 1 hour at room temperature and then the pyridine was removed by evaporation. The oil was triturated with toluene, re-evaporated and then partitioned between chloroform and saturated brine. The chloroform layer was separated and dried over magnesium sulphate, filtered off and evaporated to a clear oil which crystallised on the addition of petrol. The solid was filtered off, washed with petrol and dried to yield 0.4 g (40%) of N-pivaloyl-L-alanyl-L-proline ethylamide of melting point 94°-96° C.

WORKUP

后处理

  1. customthe pyridine was removed by evaporation
  2. customThe oil was triturated with toluene
  3. customre-evaporated
  4. custompartitioned between chloroform and saturated brine
  5. customThe chloroform layer was separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered off
  8. customevaporated to a clear oil which
  9. customcrystallised on the addition of petrol
  10. filtrationThe solid was filtered off
  11. washwashed with petrol
  12. customdried