HRID1891002

反应详情

EQUATION

反应方程式

HRID 1891002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-[2-(2-methoxy-ethoxy)-phenyl]-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (0.3 g, 1.08 mmol) is dissolved in EtOH (10 mL) and aqueous solution of ammonia (25%, 3 mL). After addition of Raney-Nickel (0.3 g) the reaction mixture is stirred under reflux for 1 h, filtered from the solid material, which is washed with a mixture of ammonia and EtOH. The combined solutions were evaporated, dissolved in water (5 mL), neutralized with 10% HCl and extracted with ethyl acetate (3×10 mL). Organic layers were combined, washed with water (5 mL) then dried over anhydrous sodium sulfate and concentrated. The residue was triturated with diethyl ether yielding 0.2 g (75%) 6-[2-(2-methoxy-ethoxy)-phenyl]-3H-pyrimidin-4-one as white powder.

WORKUP

后处理

  1. temperatureunder reflux for 1 h
  2. filtrationfiltered from the solid material, which
  3. washis washed with a mixture of ammonia and EtOH
  4. customThe combined solutions were evaporated
  5. dissolutiondissolved in water (5 mL)
  6. extractionextracted with ethyl acetate (3×10 mL)
  7. washwashed with water (5 mL)
  8. dry with materialthen dried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customThe residue was triturated with diethyl ether yielding 0.2 g (75%) 6-[2-(2-methoxy-ethoxy)-phenyl]-3H-pyrimidin-4-one as white powder