HRID485656
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
CONDITIONS
反应条件
- 温度
- 35 °C
PROCEDURE
实验过程
5-(4-Methoxybenzyl)-2-thiouracil (105 g) was refluxed in glacial acetic acid (800 ml) and 48% aqueous hydrobromic acid (400 ml) for 3 hrs. The solution was cooled to ca. 35° C., methyl iodide (53 ml) was added and the solution was refluxed for a further 2 hours. The mixture was evaporated to dryness in vacuo and water (500 ml) added to the residue. Sodium hydroxide was added to raise the pH to ca. 5. The solid which formed was filtered off and recrystallised from ethanol giving 4-hydroxybenzyl-2-methylthio-4-pyrimidone (43.1 g) m.p. 243°-4° C.
WORKUP
后处理
- temperaturethe solution was refluxed for a further 2 hours
- customThe mixture was evaporated to dryness in vacuo and water (500 ml)
- additionadded to the residue
- additionSodium hydroxide was added
- temperatureto raise the pH to ca. 5
- customThe solid which formed
- filtrationwas filtered off
- customrecrystallised from ethanol