HRID1931895

反应详情

EQUATION

反应方程式

HRID 1931895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Preparation according to preparation 4: (+)-1-benzyl-3-(2,3-difluorophenyl)pyrrolidin-3-ol (2.86 g, 9.88 mmol), ammonium formiate (1.25 g, 19.76 mmol), ethanol (50 mL) and palladium on carbon (130 mg). Refluxed for 90 min. Dichloromethane/methyl tert-butyl ether (1:1, 50 mL) was added and the mixture was filtrated through celite, the filtrate was evaporated and purified by flash column chromatography on silica gel (triethylamine/methanol, 0:1 to 1:4) to give the title compound (1.0 g). MS m/z (relative intensity, 70 eV) 199 (M+, bp), 141 (84), 113 (65), 127 (64), 63 (48).

WORKUP

后处理

  1. customPreparation
  2. customaccording to preparation 4
  3. temperatureRefluxed for 90 min
  4. filtrationthe mixture was filtrated through celite
  5. customthe filtrate was evaporated
  6. custompurified by flash column chromatography on silica gel (triethylamine/methanol, 0:1 to 1:4)