Ammonia → HCID 54274160、化合物
反応式
[CH:1]([C:3]12[CH2:9][N:6]3[CH2:7][CH:8]1[CH:4]2[CH2:5]3)=O.[C-:10]#[N:11].[K+].[NH3:13].[Cl-].[NH4+]>O>[NH2:13][CH:1]([C:3]12[CH2:9][N:6]3[CH2:7][CH:8]1[CH:4]2[CH2:5]3)[C:10]#[N:11]参加物
6
実験手順
To an icecooled solution of 1-formyl-4-azatricyclo[2.2.1.02,6 ]heptane (3.56 g, 29 mmol) in water (5 ml) was added a solution of potassium cyanide (2.08 g, 31.9 mmol) in water (5 ml) over 30 min. After an additional 1 h, cooling was removed and the reaction stirred at room temperature for 16 h. The cyanohydrin product was then added 25% aqueous ammonia (4.0 ml, 52 mmol) and ammonium chloride (7.76 g, 145 mmol). The reaction mixture was stirred at room temperature for 18 h and then extracted with isopropanole/dichloromethane (1:10) (10×75 ml). The organic phases were dried and evaporated to give the title compound as an oil (2.5 g, 58%).
後処理
- temperaturecooling
- customwas removed
- stirringThe reaction mixture was stirred at room temperature for 18 h
- extractionextracted with isopropanole/dichloromethane (1:10) (10×75 ml)
- customThe organic phases were dried
- customevaporated
出典と根拠
- ORDレコード
- ord-cc9378448944404c835f9c103736cf34
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05914338
反応ノート
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