反应详情

温度

2.5 °C

Solid BrCN 6.059 g (57.2 mmol) was added in one portion into ice-cooled slurry of (4-hydroxy-phenyl)-acetic acid hydrazide 8.642 g (52.0 mmol) and KHCO3 6.510 g (65 mmol) in MeOH (100 mL). The mixture was stirred at 0-5° C. for 1 hour, the ice bath allowed to melt and stirred at room temperature overnight (18 hr). The reaction mixture was diluted with water (100 mL), stirred for 1 hour, the precipitate was collected by filtration, washed with water and dried on high vacuum. A second fraction precipitated after concentrating and cooling the supernatants.

1. stirringstirred at room temperature overnight (18 hr)
2. stirringstirred for 1 hour
3. filtrationthe precipitate was collected by filtration
4. washwashed with water
5. customdried on high vacuum
6. customA second fraction precipitated
7. concentrationafter concentrating
8. temperaturecooling the supernatants