Sodium Cyanide → 6-Amino-4-methylnicotinonitrile
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5](Br)=[CH:4][N:3]=1.[Cu][C:11]#[N:12].[C-]#N.[Na+]>CN(C)C=O.O>[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([C:11]#[N:12])=[CH:4][N:3]=1参加物
6
実験手順
A mixture of 2-amino-5-bromo-4-methylpyridine (4.0 g, 21.4 mmol) and copper(I) cyanide (2.2 g, 24.6 mmol) in N,N-dimethylformamide (5 mL) was stirred for 4 h at reflux temperature. The hot mixture was poured into a warm solution of sodium cyanide (4.3 g) in water (13 mL). After the mixture was vigorously shaken, the mixture was extracted with ethyl acetate. The organic extract was washed with 10% aqueous sodium cyanide, saturated brine solution and evaporated. The title compound was obtained as a solid after chromatography on silica gel (15% acetone/hexane); yield 1.81 g (64%).
後処理
- temperatureat reflux temperature
- stirringAfter the mixture was vigorously shaken
- extractionthe mixture was extracted with ethyl acetate
- extractionThe organic extract
- washwas washed with 10% aqueous sodium cyanide, saturated brine solution
- customevaporated
出典と根拠
- ORDレコード
- ord-91262695ff1a4c09be98dce544f04b85
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05972975
反応ノート
読み込み中…