HRID41356

反应详情

EQUATION

反应方程式

HRID 41356 的结构方程式

PROCEDURE

实验过程

To 2-(trifluoromethyl)pyrimidin-4-ol (2 g, 12 mmol) was added POCl3 (15 mL). It was refluxed overnight. The solvent was removed. 1N NaOH was added to the reaction mixture slowly until pH=10. The mixture was extracted with DCM (3×80 mL). Combined DCM layer dried over Na2SO4 and taken to dryness. The crude product was vacuum distilled. 4-chloro-2(trifluoromethyl)pyrimidine was obtained as a clear oil. (94%). 1H NMR (400 MHz, DCM) δ: 7.60 (d, J=3 Hz, 1H), 8.80 (d, J=3 Hz, 1H),

WORKUP

后处理

  1. temperatureIt was refluxed overnight
  2. customThe solvent was removed
  3. addition1N NaOH was added to the reaction mixture slowly until pH=10
  4. extractionThe mixture was extracted with DCM (3×80 mL)
  5. dry with materialCombined DCM layer dried over Na2SO4
  6. distillationdistilled