Dimethyl Sulfate → 4-Chloro-2-nitroanisole
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-ff25cd82978a4167b74cb6d6a89e2ad9
- 출처 데이터셋
- uspto-grants-1979_01
- 특허 번호
- US04132786
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