Methylamine → 2-(Methylamino)pyridine-3-carbonitrile
反応式
Cl[C:2]1[N:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[CH3:10][NH2:11]>>[CH3:10][NH:11][C:2]1[N:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5]参加物
3
実験手順
A solution of 2-chloronicotinonitrile (97.82 g, 706 mmol) in 40% aqueous methylamine (706 ml) was heated to reflux for 1.5 hour. The excess methylamine was evaporated off and the resulting solids filtered and washed with water (250 mL). The crude product was dissolved in boiling water (1.4 1) and treated with charcoal and filtered through Celite. The aqueous filtrate was cooled to room temperature. After 10 hours the crystalline solid was collected, washed with water and dried to leave 71.10 g of 2-(methylamino)-nicotinonitrile (mp. 86-88 degrees C.). A sample was further purified by sublimation (100 degrees C. at 0.025 mm) mp. (87-88 degrees C.).
後処理
- temperatureto reflux for 1.5 hour
- customThe excess methylamine was evaporated off
- filtrationthe resulting solids filtered
- washwashed with water (250 mL)
- dissolutionThe crude product was dissolved
- additiontreated with charcoal
- filtrationfiltered through Celite
- customAfter 10 hours the crystalline solid was collected
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-8f3bc1710cbd4d06aaf3bdf45d6d7c6e
- 出典データセット
- uspto-grants-1991_03
- 特許番号
- US05002944
反応ノート
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