反应详情

A mixture of 3-methyl-1H-pyrazol-5-amine (0.186 g, 1.92 mmol) and acetic acid (3.71 mL, 65.2 mmol) was slightly heated until complete dissolution and the resultant solution was cooled to RT and mixed with ethyl 2-bromo-3-oxobutanoate (1.20 g, 5.74 mmol). The resultant reaction mixture was stirred at RT for 16 h, after which time the reaction mixture was diluted with diethyl ether, cooled to 0° C. and stirred at that temperature for 30 min. The white solid precipitate was separated by filtration and washed with cold diethyl ether and dried to give the desired product (363 mg, 78%) as a white solid. LCMS calculated for C8H9BrN3O (M+H)+: m/z=242.0, 244.0. found: 241.9, 244.0.

1. temperaturewas slightly heated until complete dissolution
2. customThe resultant reaction mixture
3. temperaturecooled to 0° C.
4. stirringstirred at that temperature for 30 min
5. customThe white solid precipitate was separated by filtration
6. washwashed with cold diethyl ether
7. customdried