HRID41356
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureIt was refluxed overnight
- customThe solvent was removed
- addition1N NaOH was added to the reaction mixture slowly until pH=10
- extractionThe mixture was extracted with DCM (3×80 mL)
- dry with materialCombined DCM layer dried over Na2SO4
- distillationdistilled