HRID639086

反应详情

EQUATION

反应方程式

HRID 639086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of (±)-1,1-dimethylethyl trans-3-hydroxy-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate (4.44 g, 12.7 mmole) in DCM (75 mL) was added TFA (25 mL). After stirring for 2 h, the reaction contents were concentrated under vacuum and the residue dissolved in DCM (150 mL). MP-carbonate resin (18.8 g, 50.8 mmole) was added and the reaction contents were stirred vigorously overnight. The reaction contents were filtered through a scinter-glass funnel and the resin washed with MeOH. The filtrate was concentrated and dried under vacuum to give an off-white foam: LC-MS (ES) m/e 251 (M+H)+.

WORKUP

后处理

  1. customthe reaction contents
  2. concentrationwere concentrated under vacuum
  3. dissolutionthe residue dissolved in DCM (150 mL)
  4. customthe reaction contents
  5. stirringwere stirred vigorously overnight
  6. customThe reaction contents
  7. filtrationwere filtered through a scinter-glass funnel
  8. washthe resin washed with MeOH
  9. concentrationThe filtrate was concentrated
  10. customdried under vacuum
  11. customto give an off-white foam