HRID1110041

反应详情

EQUATION

反应方程式

HRID 1110041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirred solution of spiro[indane-1,4'-piperidine] (110 mg, 0.59 mmol), in anhydrous DMF (10 ml), under an atmosphere of nitrogen, was added potassium carbonate (98 mg, 0.71 mmol) followed by benzyl bromide (0.08 ml, 0.65 mmol) dropwise. The mixture was heated at 100° C. for 2 hours, after which time the solution was cooled to ambient temperature. The solvent was removed in vacuo, then ether (20 ml) was added to the residue and the mixture was washed with water (2×20 ml). The organic layer was separated, dried (MgSO4) and the solvent evaporated in vacuo. The crude residue was chromatographed using 1:1 petrol (60/80):ether, to give 1'-benzylspiro[indane-1,4'-piperidine] as a viscous colourless oil (31 mg, 20%).

WORKUP

后处理

  1. temperatureafter which time the solution was cooled to ambient temperature
  2. customThe solvent was removed in vacuo
  3. additionether (20 ml) was added to the residue
  4. washthe mixture was washed with water (2×20 ml)
  5. customThe organic layer was separated
  6. dry with materialdried (MgSO4)
  7. customthe solvent evaporated in vacuo
  8. customThe crude residue was chromatographed