反应 #1605751

ord-2ee85b796fca44e285d8cc656a2efa0a

反应方程式

CCCC(=O)CC(C)C
2-methylheptan-4-one
CC(=O)[O-].[NH4+]
ammonium acetate
[BH3-]C#N.[Na+]
sodium cyanoborohydride
CCCC(N)CC(C)C
2-methylheptan-4-amine
收率 77.2%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe residue was diluted with water and basified with 15% NaOH aqueous
  3. 3
    萃取extracted with ether
  4. 4
    洗涤The extract was washed with brine
  5. 5
    干燥dried over anhydrous magnesium sulfate
  6. 6
    过滤filtered
  7. 7
    其他evaporated

实验过程

To a solution of 2-methylheptan-4-one (4.24 g, 33.07 mmol), in methanol (60 mL), were added ammonium acetate (25.50 g, 330.71 mmol) and sodium cyanoborohydride (2.08 g, 33.07 mmol). The reaction mixture was stirred at room temperature for about 24 hours. The solvent was removed under reduced pressure and the residue was diluted with water and basified with 15% NaOH aqueous and extracted with ether. The extract was washed with brine, dried over anhydrous magnesium sulfate, filtered and evaporated to give 3.3 g of 2-methylheptan-4-amine (77%). MS (M+H, 130).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09072313B2uspto-grants-2015_07