反応 #1605751

ord-2ee85b796fca44e285d8cc656a2efa0a

反応方程式

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
収率 77.2%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe residue was diluted with water and basified with 15% NaOH aqueous
  3. 3
    抽出extracted with ether
  4. 4
    洗浄The extract was washed with brine
  5. 5
    乾燥dried over anhydrous magnesium sulfate
  6. 6
    ろ過filtered
  7. 7
    その他evaporated

実験手順

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).

出典

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