HRID232550

反应详情

EQUATION

反应方程式

HRID 232550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 8-t-butyl-3-aminomethyl-1-oxaspiro(4,5)-decane (1.2 g, 5.3 mmol), cyclohexanone (0.54 g, 5.5 mmol) and zinc chloride (0.4 g, 3 mmol) in methanol (15 ml) was added sodium cyanoborohydride (0.4 g, 6.4 mmol). The reaction mixture was stirred over night. The solvent was then evaporated in vacuo and the resulting residue was treated with a mixture of saturated aqueous sodium carbonate/toluene (50 ml each). The organic layer was separated, dried (MgSO4) and evaporated in vacuo to yield 1.7 g of a pale yellow oil which was purified by flash chromatography (toluene/ethanol 4:1). Evaporation of the fractions containing the product yielded a colourless oil (1.5 g).

WORKUP

后处理

  1. customThe solvent was then evaporated in vacuo
  2. additionthe resulting residue was treated with a mixture of saturated aqueous sodium carbonate/toluene (50 ml each)
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. customevaporated in vacuo