HRID1670621

反应详情

EQUATION

反应方程式

HRID 1670621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the (3S,4R)-tert-butyl 3-(4-bromo-2-nitrophenylamino)-4-(2-chloroacetoxy)pyrrolidine-1-carboxylate (2.20 mmol, 1.0 g) in methanol add 2.0 M aqueous lithium hydroxide (5 mL) and stir at room temperature for 3.5 h. Remove the solvent, dilute the residue with ethyl acetate (50 mL), and wash with water and brine. Dry over anhydrous sodium sulfate, filter, and evaporate the solvent. Purify by column chromatography eluting with 50% ethyl acetate in methylene chloride to obtain the title compound as a yellow solid (900 mg, 98%). APCI MS m/z 462 [M+H]+.

WORKUP

后处理

  1. customRemove the solvent
  2. additiondilute the residue with ethyl acetate (50 mL)
  3. washwash with water and brine
  4. dry with materialDry over anhydrous sodium sulfate
  5. filtrationfilter
  6. customevaporate the solvent
  7. customPurify by column chromatography
  8. washeluting with 50% ethyl acetate in methylene chloride