HRID2117733

反应详情

EQUATION

反应方程式

HRID 2117733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(4-Fluorophenyl)-1-pyridin-4-ylethanone (0.04 mol/8.6 g) (prepared as described in example 20, steps (a) and (b)) was dissolved in 80 ml of glacial acetic acid. NaNO2 (0.04 mol/2.76 g), dissolved in the smallest amount of H2O possible, was then added dropwise with ice-cooling and stirring. The mixture was then stirred at 0° C. for another 2 h. 500 ml of H2O were then added, and the mixture was stirred at room temperature for another 1 h. The title compound precipitated as a white powder. The precipitate was filtered off, washed with H2O and dried over P2O5 under reduced pressure. Yield: 5.9 g (60%)

WORKUP

后处理

  1. additionwas then added dropwise with ice-
  2. temperaturecooling
  3. stirringThe mixture was then stirred at 0° C. for another 2 h
  4. stirringthe mixture was stirred at room temperature for another 1 h
  5. customThe title compound precipitated as a white powder
  6. filtrationThe precipitate was filtered off
  7. washwashed with H2O
  8. dry with materialdried over P2O5 under reduced pressure