HRID1969749

反应详情

EQUATION

反应方程式

HRID 1969749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Ethyl 4-(dibenzylamino)-2-methylcyclopentanecarboxylate (3.65 g, 10.38 mmol) was dissolved in a mixture of HCl (6 N aqueous, 20 mL) and 1,4-dioxane (50 mL) and the resulting mixture was heated at about 60° C. for about 72 h. The organic solvent was removed under reduced pressure. The aqueous phase was neutralized by the addition of saturated aqueous NaHCO3 (40 mL) and extracted with EtOAc (50 mL). The organic phase was washed with brine (40 mL), dried over anhydrous MgSO4 and concd under reduced pressure to yield 4-(dibenzylamino)-2-methylcyclopentanecarboxylic acid (3.3 g, 98%) as a white amorphous solid: LC/MS (Table 1, Method a) Rt=1.66 min; MS m/z 324 (M+H)+.

WORKUP

后处理

  1. customThe organic solvent was removed under reduced pressure
  2. additionThe aqueous phase was neutralized by the addition of saturated aqueous NaHCO3 (40 mL)
  3. extractionextracted with EtOAc (50 mL)
  4. washThe organic phase was washed with brine (40 mL)
  5. dry with materialdried over anhydrous MgSO4 and concd under reduced pressure