Ammonium Acetate → HCID 68292043、化合物
反応式
[CH3:1][C:2]1([C:8]#[N:9])[CH2:6][CH2:5][CH2:4][C:3]1=O.C([O-])(=O)C.[NH4+].C([BH3-])#[N:16].[Na+]>CO>[NH2:16][CH:3]1[CH2:4][CH2:5][CH2:6][C:2]1([CH3:1])[C:8]#[N:9]参加物
5
実験手順
A mixture of 1-methyl-2-oxocyclopentanecarbonitrile (272 mg, 2.209 mmol, from Step 1) and ammonium acetate (917 mg, 11.90 mmol) in methanol (2 mL) was stirred at room temperature for 2 h. Sodium cyanoborohydride (69.4 mg, 1.104 mmol) was added. After 17 h at room temperature, the mixture was concentrated. The residue was dissolved in water and ethyl acetate and stirred vigorously. The ethyl acetate phase was separated, dried (MgSO4), filtered and concentrated to give crude 2-amino-1-methylcyclopentanecarbonitrile (0.2436 g), which was taken to the next reaction without purification.
後処理
- waitAfter 17 h at room temperature
- concentrationthe mixture was concentrated
- dissolutionThe residue was dissolved in water
- stirringethyl acetate and stirred vigorously
- customThe ethyl acetate phase was separated
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-59c2f0a170244aaca3b11bd2d9b93815
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921368B2
反応ノート
読み込み中…