HRID30230

反应详情

EQUATION

反应方程式

HRID 30230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Trifluoroacetic acid (10 ml) was added to 2,5-diphenylpyrrolidine (1.01 g, 3.13 minol) at 0° C. The mixture was stirred at 0° C. for 10 minutes, then the solvent was evaporated to afford a light brown solid to which was added 100 ml of water. To this solution was added 1N NaOH until pH=14 and the aqueous phase was extracted with chloroform. The organic phase was washed with 1N NaOH, water, brine and dried over MgSO4. After filtration and evaporation to dryness, the light-yellow solid obtained was dissolved in diethyl-ether. To this solution was added IN HCl (5 ml, 5 mmol), the precipitate obtained was collected by filtration, washed with diethyl-ether and dried under vacuum (0.590 g, 72.7%). 1H-NMR (CDCl3): δ ppm 7.30-7.60 (m, ArH, 10H), 4.95 (m, ArCH, 2H), 2.45-2.70 (m, CH2, 4H).

WORKUP

后处理

  1. customthe solvent was evaporated
  2. customto afford a light brown solid to which
  3. extractionthe aqueous phase was extracted with chloroform
  4. washThe organic phase was washed with 1N NaOH, water, brine
  5. dry with materialdried over MgSO4
  6. filtrationAfter filtration and evaporation to dryness
  7. customthe light-yellow solid obtained
  8. customthe precipitate obtained
  9. filtrationwas collected by filtration
  10. washwashed with diethyl-ether
  11. customdried under vacuum (0.590 g, 72.7%)