HRID2235193

反应详情

EQUATION

反应方程式

HRID 2235193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dissolve cis-4-nitro-benzoic acid 4-(2-oxo-pyrrolidin-1-yl)-cyclohexyl ester (Preparation 15) (87.9 g; 264 mmol) in methanol (1.35 L) and water (150 mL) and add potassium carbonate (109.5 g; 800 mmol). Stir at room temperature overnight to give a white precipitate. Evaporate to dryness. Azeotrope with ethanol (×2). Stir in tetrahydrofuran (1 L) for 1 hour then filter. Evaporate the filtrate to an oil and crystallize from diethyl ether (100 mL) to afford 40 g (83%) of the title compound.

WORKUP

后处理

  1. customto give a white precipitate
  2. customEvaporate to dryness
  3. stirringStir in tetrahydrofuran (1 L) for 1 hour
  4. filtrationthen filter
  5. customEvaporate the filtrate to an oil
  6. customcrystallize from diethyl ether (100 mL)