HRID1708517
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
1.06 g (6 mmol) of 5-methyl-4-(1,2,4-triazol-1-yl)-pyrimidin-2(1H)-one are boiled under reflux with 972 mg (18 mmol) of sodium methylate in 30 ml of anhydrous methanol for 4 hours with exclusion of moisture. The cooled solution is neutralized with acetic acid, concentrated and chromatographed on silica gel using ethyl acetate/methanol 9/1. 770 mg (91.7% of theory) of 4-methoxy-5-methylpyrimidin-2(1H)-one are obtained with melting point 196°-199° C. 1H NMR (270 MHz, d6 -DMSO), δ[ppm]: 11.09 (s, 1H), 7.51 (d, 1H), 3.83 (s, 3H), 1.85 (s, 3H).
WORKUP
后处理
- concentrationconcentrated
- customchromatographed on silica gel