HRID900741
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
A mixture of 6-chloro-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione (3.76 g), sodium hydrosulphide hydrate (6.0 g) and ethanol (100 ml) was stirred at room temperature for 48 h then concentrated under reduced pressure. The residue was dissolved in water (500 ml) and washed with ethyl acetate (2×100 ml). The aqueous phase was acidified with dilute hydrochloric acid, then extracted with ethyl acetate (3×100 ml). The combined organic phase was dried (MgSO4) and concentrated in vacuo to give a pale yellow solid which was used directly in the next step.
WORKUP
后处理
- concentrationthen concentrated under reduced pressure
- dissolutionThe residue was dissolved in water (500 ml)
- washwashed with ethyl acetate (2×100 ml)
- extractionextracted with ethyl acetate (3×100 ml)
- dry with materialThe combined organic phase was dried (MgSO4)
- concentrationconcentrated in vacuo
- customto give a pale yellow solid which