HRID2233112

反应详情

EQUATION

反应方程式

HRID 2233112 的结构方程式

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

  1. temperaturewas heated
  2. customwas consumed
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux for about 2 h
  5. temperaturecooled to ambient temperature
  6. custompartitioned between EtOAc and water
  7. customThe layers were separated
  8. dry with materialthe organic phase was dried over MgSO4
  9. filtrationfiltered
  10. customevaporated
  11. customThe resulting solid was triturated with heptane