反応式
[CH3:1][C:2]1[C:7]([NH:8][C:9](=[O:12])[CH2:10]Cl)=[CH:6][CH:5]=[C:4]([CH3:13])[N:3]=1.[P:14]([O-:26])([O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)([O:16][CH3:17])=[O:15].[K+].CC(C)=O>CCOCC>[P:14]([O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)([O:16][CH3:17])([O:26][CH2:10][C:9]([NH:8][C:7]1[C:2]([CH3:1])=[N:3][C:4]([CH3:13])=[CH:5][CH:6]=1)=[O:12])=[O:15]参加物
5
実験手順
N-(2,6-Dimethyl-3-pyridyl)-α-chloroacetamide (32.2 grams), potassium O-methyl O-(4-chlorophenyl) phosphate (26 grams) and acetone (200 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is heated at reflux for a period of about 24 hours. After this time the mixture is stripped of solvent on a steam bath and the resulting residue is dissolved in ether. The ether solution is washed with water and is dried over magnesium sulfate. The dried solution is then evaporated under vacuum to yield the desired product O-[2-(2,6-dimethyl-3-pyridylamino)-2-ketoethyl] O-methyl O-(4-chlorophenyl) phosphate.
後処理
- customequipped with a mechanical stirrer
- temperaturethermometer and reflux condenser
- temperatureThe reaction mixture is heated
- temperatureat reflux for a period of about 24 hours
- customAfter this time the mixture is stripped of solvent on a steam bath
- washThe ether solution is washed with water
- dry with materialis dried over magnesium sulfate
- customThe dried solution is then evaporated under vacuum
出典と根拠
- ORDレコード
- ord-9a4d6d8b58a642e29525e9cf6126711e
- 出典データセット
- uspto-grants-1976_12
- 特許番号
- US03996352
関連ノート
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