HRID1590492

反应详情

EQUATION

反应方程式

HRID 1590492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2S,4S)-2-azidomethyl-1-(4-nitrobenzyloxycarbonyl)-4-(triphenylmethylthio)pyrrolidine (5.18 g) and triphenylphosphine (3.75 g) in pyridine (15 ml) was stirred at ambient temperature for 1 hour. To a reaction mixture was added conc. ammonia water (1.2 ml) with stirring at ambient temperature and the mixture was allowed to stand overnight at the same temperature. The solution was evaporated in vacuo to give a residue. The residue was chromatographed on silica gel (100 g) eluting with a mixture of chloroform and methanol (9:1, V/V). The fractions containing the desired compound were collected and evaporated in vacuo to give (2S,4S)-2-aminomethyl-1-(4-nitrobenzyloxycarbonyl)-4-(triphenylmethylthio)pyrrolidine (6.13 g).

WORKUP

后处理

  1. customThe solution was evaporated in vacuo
  2. customto give a residue
  3. customThe residue was chromatographed on silica gel (100 g)
  4. washeluting with a mixture of chloroform and methanol (9:1, V/V)
  5. additionThe fractions containing the desired compound
  6. customwere collected
  7. customevaporated in vacuo