HRID1853036

反应详情

EQUATION

反应方程式

HRID 1853036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask charged with tert-butyl 4-(4-(5-hydroxyimidazo[1,2-c]pyrimidin-7-yl)phenyl)piperidine-1-carboxylate (1.75 g, 4.44 mmol) in 40 mL of dichloromethane was added 2,2,2-trifluoroacetic acid (15 mL, 195 mmol) at ambient temperature for 3 hours. The solvent was concentrated under reduced pressure and the resulting crude was taken up in methanol (10 mL) and to it was added aqueous saturated sodium bicarbonate slowly. The resulting solid was collected by means of vacuum filtration and was dried overnight on high vacuum. This solid was triturated with water (50 mL) and solids were collected by means of vacuum filtration and dried on high vacuum to afford 7-(4-(piperidin-4-yl)phenyl)imidazo[1,2-c]pyrimidin-5-ol (1.03 g, 3.50 mmol, 78.9% yield). MS (apci) m/z=295.1 (M+H).

WORKUP

后处理

  1. concentrationThe solvent was concentrated under reduced pressure
  2. additionwas added aqueous saturated sodium bicarbonate slowly
  3. filtrationThe resulting solid was collected by means of vacuum filtration
  4. customwas dried overnight on high vacuum
  5. customThis solid was triturated with water (50 mL) and solids
  6. filtrationwere collected by means of vacuum filtration
  7. customdried on high vacuum