HRID1590505

反应详情

EQUATION

反应方程式

HRID 1590505 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of (2S,4R)-4-methanesulfonyloxy-2-(2-oxoimidazolidin-1-yl)carbonylpyrrolidine (14.9 g) in a mixture of methanol (150 ml) and tetrahydrofuran (150 ml) were added triethylamine (32.5 ml) and methyl iodide (11.4 ml) and the mixture was stirred at 40° C. for 2 hours. The reaction mixture was evaporated in vacuo. The resulting residue was chromatographed on silica gel (600 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 a residue. The residue was washed with dichloromethane (100 ml). The resulting precipitates were collected and dried in vacuo to give (2S,4R)-4-methanesulfonyloxy-1-methyl-2-(2-oxoimidazolidin-1-yl)carbonylpyrrolidine (2.30 g).

WORKUP

后处理

  1. customThe reaction mixture was evaporated in vacuo
  2. customThe resulting residue was chromatographed on silica gel (600 g)
  3. washeluting with a mixture of chloroform and methanol (9:1 V/V)
  4. additionThe fractions containing the desired compound
  5. customwere collected
  6. customevaporated in vacuo
  7. customto give a residue
  8. washThe residue was washed with dichloromethane (100 ml)
  9. customThe resulting precipitates
  10. customwere collected
  11. customdried in vacuo