反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of anhydrous IPA (25 mL) and sodium (0.4 g, 17.4 mmol) was heated at reflux until the sodium was consumed. The reaction mixture was cooled to ambient temperature and the 8-chloro-2-(4-fluorophenyl)-imidazo[1,2-a]pyrazine (prepared from general procedure B using 3-chloropyrazin-2-ylamine and 2-bromo-1-(4-fluorophenyl)-ethanone; 2.0 g, 8 mmol) was added. The reaction mixture was heated at reflux for about 2 h, cooled to ambient temperature, and partitioned between EtOAc and water. The layers were separated and the organic phase was dried over MgSO4, filtered, and evaporated. The resulting solid was triturated with heptane to afford 1.52 g (70%) of the title compound: LC/MS (Table 1, Method g) Rt=2.78 min; MS m/z: 272.2 (M+H)+.
WORKUP
后处理
- temperaturewas heated
- customwas consumed
- temperatureThe reaction mixture was heated
- temperatureat reflux for about 2 h
- temperaturecooled to ambient temperature
- custompartitioned between EtOAc and water
- customThe layers were separated
- dry with materialthe organic phase was dried over MgSO4
- filtrationfiltered
- customevaporated
- customThe resulting solid was triturated with heptane