Dimethyl Sulfate → 4-Chloro-2-nitroanisole
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[C:12](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:12])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1参加物
5
実験手順
0.072 mol (12.6 g) of 4-chloro-2-nitrophenol, 40 ml of acetone and 9.72 g of potassium carbonate are introduced into a 250 ml three-necked flask equipped with a stirring system, a thermometer and a condenser. The mixture is brought to 40° C. and 9.72 g of dimethyl sulphate are then added drop by drop; the mixture is heated under reflux for 5 hours; the potassium sulphate is separated; the acetone solution is concentrated under reduced pressure and the 4-chloro-2-nitroanisole is precipitated. It is separated and then crystallized in a water/acetone mixture.
後処理
- customequipped with a stirring system
- customis brought to 40° C.
- temperaturethe mixture is heated
- temperatureunder reflux for 5 hours
- customthe potassium sulphate is separated
- concentrationthe acetone solution is concentrated under reduced pressure
- customthe 4-chloro-2-nitroanisole is precipitated
- customIt is separated
- customcrystallized in a water/acetone mixture
出典と根拠
- ORDレコード
- ord-84f8493b1e3d454485e7ff009f8de7aa
- 出典データセット
- uspto-grants-1980_07
- 特許番号
- US04211776
反応ノート
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