HRID346340

反应详情

EQUATION

反应方程式

HRID 346340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2S,4R)-4-t-butyldimethylsilyloxy-2-(carbamoylmethyl)thiomethyl-1-(4-nitrobenzyloxycarbonyl)pyrrolidine (2.10 g) in methanol (40 ml) was added conc. hydrochloric acid (0.72 ml) at ambient temperature After stirring at the same temperature for 1 hour, this reaction mixture was concentrated under reduced pressure to give a residue. The residue was dissolved in ethyl acetate (60 ml). The solution was washed with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride successively, dried over anhydrous magnesium sulfate, and evaporated in vacuo to give a residue. The residue was washed with a mixture of ethyl acetate (30 ml) and diisopropyl ether (15 ml). The resulting precipitates were collected by filtration and air-dried to give (2S,4R)-2-(carbamoylmethyl)thiomethyl-4-hydroxy-1-(4-nitrobenzyloxycarbonyl)pyrrolidine (1.08 g).

WORKUP

后处理

  1. concentrationthis reaction mixture was concentrated under reduced pressure
  2. customto give a residue
  3. washThe solution was washed with saturated aqueous sodium hydrogen carbonate and saturated aqueous sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated in vacuo
  6. customto give a residue
  7. washThe residue was washed with a mixture of ethyl acetate (30 ml) and diisopropyl ether (15 ml)
  8. customThe resulting precipitates
  9. filtrationwere collected by filtration
  10. customair-dried