HRID412010

反应详情

EQUATION

反应方程式

HRID 412010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product from step (b) (0.7 g) and 1,1′-carbonyldiimidazole (0.62 g) were dissolved in N,N-dimethylformamide (10 ml) and stirred at room temperature for 1 hour. tert-Butyl 4-(2-aminoethyl)-1-piperazinecarboxylate (2.73 g) was added, the solution stirred for 16 hours and then evaporated to leave a gum. Dichloromethane and sodium bicarbonate solution were added, the organic phase was separated, dried and concentrated to a gum which was purified by chromatography (ethyl acetate:triethylamine, 10:1) to give the product as a solid (0.62 g), m.p. 139-140° C.

WORKUP

后处理

  1. stirringthe solution stirred for 16 hours
  2. customevaporated
  3. customto leave a gum
  4. customthe organic phase was separated
  5. customdried
  6. concentrationconcentrated to a gum which
  7. customwas purified by chromatography (ethyl acetate:triethylamine, 10:1)