Sodium Cyanide → 3,5-Dimethylpyridine-2-carbonitrile
反応式
[C-:1]#[N:2].[Na+].COS([O-])(=O)=O.CO[N+:12]1[CH:17]=[C:16]([CH3:18])[CH:15]=[C:14]([CH3:19])[CH:13]=1>O>[C:1]([C:13]1[C:14]([CH3:19])=[CH:15][C:16]([CH3:18])=[CH:17][N:12]=1)#[N:2]参加物
4
実験手順
To a cooled (0° C.) solution of NaCN (49.0 g, 0.999 mol, 3.0 eq.) in 135 mL of water (air free) was dripped 1-methoxy-3,5-dimethyl pyridinium methyl sulfate (83.0 g, 0.33 mol) in 100 mL water (air free) in 1.25 hr., keeping the temperature below 3° C. The reaction mixture was stored at about 3° C. overnight. The mixture was filtered and washed with water to give 40 g of the title compound. An analytical sample was recrystallized from isopropyl ether and pentane (4:1) (m.p.: 61-62° C.).
後処理
- customin 1.25 hr
- customthe temperature below 3° C
- filtrationThe mixture was filtered
- washwashed with water
出典と根拠
- ORDレコード
- ord-4737ff8c3a9b4839b21b3b4a2a7cbf50
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06300338B1
反応ノート
読み込み中…