反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([OH:11])=[O:10])=[CH:5][CH:4]=1.[CH2:12]([NH:14][CH2:15][CH3:16])[CH3:13]>C(#N)C>[CH2:12]([N:14]([CH2:15][CH3:16])[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([OH:11])=[O:10])=[CH:5][CH:4]=1)[CH3:13]参加物
4
実験手順
1 g (1 equivalent) of α-chloroparatoluic acid and 1.22 mL (2 equivalents) of diethylamine are placed in solution in 30 mL of acetonitrile. The reaction mixture is taken to reflux for 48 hours. The solvent is evaporated off under vacuum and the residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40 then pure MeOH). The product is obtained in the form of a white powder after precipitation from hexane. (Yield=63%).
後処理
- temperatureto reflux for 48 hours
- customThe solvent is evaporated off under vacuum
- customthe residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40
- customThe product is obtained in the form of a white powder
- customafter precipitation from hexane
出典と根拠
- ORDレコード
- ord-67b3606ed97745088224a32eb7d53c20
- 出典データセット
- uspto-grants-2005_12
- 特許番号
- US06972343B1
関連ノート
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