Ethanol → HCID 20031313、化合物
反応式
C(O)C.[C-:4]#[N:5].[Na+].CS(O[CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]1[N:18]([CH3:20])[CH3:19])(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>Cl.C(Cl)Cl>[CH3:19][N:18]([CH3:20])[CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH:12]1[C:4]#[N:5]参加物
7
実験手順
To 200 mL of 80% aqueous ethanol add 10 g (0.2 mol) of sodium cyanide and 22.1 (0.1 mol) of 2-(dimethylamino)-cyclohexanol methanesulfonate. Reflux the reaction and monitor by thin-layer chromatography. Upon completion add in HCl until gas evolution ceases. Remove solvent in vacuo and add saturated aqueous sodium carbonate (ph=11) and 100 mL of methylene chloride. Separate the layers and dry the organic phase over Na2SO4. Filter the drying agent and evaporate the solvent in vacuo to obtain the title compound.
後処理
- temperatureReflux
- customthe reaction and monitor by thin-layer chromatography
- customSeparate the layers
- dry with materialdry the organic phase over Na2SO4
- filtrationFilter the drying agent
- customevaporate the solvent in vacuo
出典と根拠
- ORDレコード
- ord-ba73145d2de24935b28401061273276b
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04851526
反応ノート
読み込み中…