反应详情

A mixture of 2-amino-isonicotinic acid methyl ester (5 g, 32 mmol), ω-bromoacetophenone (6.47 g, 32 mmol), NaHCO3 (2.95 g, 35 mmol) and methanol (30 ml) was heated under an atmosphere of argon to reflux (3 h). After cooling, water (20 ml) was added, the mixture was stirred at r.t. (15 min), and filtered. The obtained solid was washed (water, methanol, diethyl ether) and dried under vacuum. The product (6.8 g, 85%) was used in the next step without further purification. MS (m/e)=253.2 [M+H+].

1. temperaturewas heated under an atmosphere of argon
2. temperatureto reflux (3 h)
3. temperatureAfter cooling
4. filtrationfiltered
5. washThe obtained solid was washed (water, methanol, diethyl ether)
6. customdried under vacuum
7. customThe product (6.8 g, 85%) was used in the next step without further purification