HRID1755850
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationAfter a further 4 hours at 60° C. the mixture is filtered
- concentrationthe filtrate is concentrated
- dissolutionThe residue is dissolved in about 150 ml of water
- filtrationThe precipitated product is filtered off under suction
- washwashed with water
- customdried at room temperature
- customcrystallized from ethanol