Hydrochloric Acid → 4-Hydroxy-1-methylpiperidine-4-carbonitrile
反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.Cl.[C-:10]#[N:11].[K+]>O>[OH:8][C:5]1([C:10]#[N:11])[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1参加物
5
反応条件
- 温度
- 10 °C
実験手順
To freshly distilled 1-methylpiperidin-4-one (81.72 g, 0.72 mole) in water (200 cc), were added about 100 cc HCl 37% to pH 3. The reaction mixture was cooled in an ice bath and potassium cyanide (49 g, 0.75 mole) in water (200 cc) was added at an adequate rate in order to maintain an internal temperature of about 10° C. The reaction was stirred two hours more after the addition and then filtered. After washing with water and drying, the product, 4-hydroxy-4-cyano-1-methylpiperidine, was obtained in 67% yield as a white powder (67 g, 0.48 mole, mp. 135° C.).
後処理
- temperatureThe reaction mixture was cooled in an ice bath
- additionmore after the addition
- filtrationfiltered
- washAfter washing with water
- customdrying
出典と根拠
- ORDレコード
- ord-eb0b82aade02403387005403ea3040cf
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05534520
反応ノート
読み込み中…