反应详情

To a stirred solution of N-(5-Bromo-pyridin-2-yl)-acetamide (1 g, 4.6 mmol) in 30 ml CH3CN was added ClCF2COONa (848 mg, 5.58 mmol), followed by 18-Crown-6 (244 mg, 0.93 mmol). The reaction mixture was heated to reflux for 12 hrs. Then the reaction mixture was cooled down and the solvent was removed under reduced pressure. To this was added methylene dichloride and washed with water. Organic layer was dried over any sodium sulphate and concentrated under reduced pressure to furnish the crude N-[5-Bromo-1-difluoromethyl-1H-pyridin-(2E)-ylidene]-acetamide. This was carried to the next step without purification.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 12 hrs
3. temperatureThen the reaction mixture was cooled down
4. customthe solvent was removed under reduced pressure
5. additionTo this was added methylene dichloride
6. washwashed with water
7. dry with materialOrganic layer was dried over any sodium sulphate
8. concentrationconcentrated under reduced pressure