HRID1755850

反应详情

EQUATION

反应方程式

HRID 1755850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(4-Chloro-2-phenyl-5-pyrimidinyl)-o-phenylene diacetate (6.0 g) (15.7 mmol) are suspended in 200 ml of methanol. 10 g of sodium hydrogen sulphide hydrate are added at 50° C. while stirring. After a further 4 hours at 60° C. the mixture is filtered and the filtrate is concentrated. The residue is dissolved in about 150 ml of water and the solution is brought to pH 5 with 1N aqueous hydrochloric acid. The precipitated product is filtered off under suction, washed with water, dried at room temperature and crystallized from ethanol. There are obtained 3.6 g of 5-(3,4-dihydroxyphenyl)-2-phenyl-4(3H)-pyrimidinethione as yellow crystals of m.p. 220° C.

WORKUP

后处理

  1. filtrationAfter a further 4 hours at 60° C. the mixture is filtered
  2. concentrationthe filtrate is concentrated
  3. dissolutionThe residue is dissolved in about 150 ml of water
  4. filtrationThe precipitated product is filtered off under suction
  5. washwashed with water
  6. customdried at room temperature
  7. customcrystallized from ethanol