HRID1976051

反应详情

EQUATION

反应方程式

HRID 1976051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To phosphorous oxychloride (2.02 ml, 21.6 mmol) was added quinoline (1.34 ml, 11.2 mmol) followed by 3-bromo-2-hydroxy-5-trifluoromethylpyridine (5.0 g, 20.7 mmol), and the mixture formed heated at 120° C. for 3 hrs. It was then cooled to 100° C. and water (10 ml) added. After cooling to 22° C., sodium hydrogen carbonate solution (100 ml) was added and the mixture extracted with ethyl acetate (2×100 ml). The extracts were dried (MgSO4) and concentrated, and the residue purified by silica chromatography to give the product as an oil (4.05 g, 75% yield).

WORKUP

后处理

  1. customthe mixture formed
  2. temperatureIt was then cooled to 100° C.
  3. temperatureAfter cooling to 22° C.
  4. extractionthe mixture extracted with ethyl acetate (2×100 ml)
  5. dry with materialThe extracts were dried (MgSO4)
  6. concentrationconcentrated
  7. customthe residue purified by silica chromatography