HRID450085

反应详情

EQUATION

反应方程式

HRID 450085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,1,2,2-Tetrafluoro-3-iodo propane (0.5 g, 2 mmol) was added to a mixture of 5-nitro-2-hydroxy pyridine (860 mg, 6.1 mmol) and potassium carbonate (1.4 g, 10 mmol) in DMF (10 ml) and the reaction heated at reflux for 6 hr. The reaction mixture was cooled to room temperature and filtered. The filtrate was diluted with ethyl acetate (50 ml), washed successively with bicarbonate solution, water, brine, and dried. Concentration to dryness yielded 5-nitro-2-(2,2,3,3-tetrafluoro-propoxy)pyridine (394 mg, 75%) as an oil.

WORKUP

后处理

  1. temperaturethe reaction heated
  2. temperatureat reflux for 6 hr
  3. filtrationfiltered
  4. additionThe filtrate was diluted with ethyl acetate (50 ml)
  5. washwashed successively with bicarbonate solution, water, brine
  6. customdried
  7. concentrationConcentration to dryness