反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
5-(6-methoxy-pyridin-3-ylmethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (395 mg, 1.58 mmol, 1 eq) was refluxed in an acetic acid, glacial (5 ml)/HCl conc. (5 ml) mixture for 16 hours. (150° C. on display of heating device). Solvent from the mixture was evaporated as much as possible. In the mixture was added 10 ml of water. pH of the mixture was adjusted to 4-5. The resulting precipitate was collected and was dried. It was obtained 5-(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (285 mg, yield=61.3%, purity=90%) in form of grey powder. MS: [M+H]+=236.20 1H NMR (300 MHz; DMSO-d6) δ/ppm 3.24 (s, 2H), 6.25 (d, J=9.36 Hz, 1H), 7.28-7-36 (m, 2H), 11.39 (br.s, 1H), 12.23 (br.s, 1H), 12.46 (br.s, 1H)
WORKUP
后处理
- customSolvent from the mixture was evaporated as much as possible
- additionIn the mixture was added 10 ml of water
- customThe resulting precipitate was collected
- customwas dried