反应详情

Dissolve 1-methyl-5-aminopyrazole (Butt Park LTD; 1.0 g, 10.3 mmol) and 2-bromomalonaldehyde (Aldrich; 1.55 g, 10.3 mmol) in glacial acetic acid (160 mL) and reflux under nitrogen for 48 h. Concentrate under reduced pressure and purify via chromatography (silica gel, 90% dichloromethane/10% diethyl ether) to obtain 610 mg (27%) of the title compound as an off-white solid. TOF MS ES+ exact mass calculated for C7H7N3Br (p+H): m/z=211.9823, Found: 211.9838.

1. temperaturereflux under nitrogen for 48 h
2. concentrationConcentrate under reduced pressure
3. custompurify via chromatography (silica gel, 90% dichloromethane/10% diethyl ether)