HRID485656

反应详情

EQUATION

反应方程式

HRID 485656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe solution was refluxed for a further 2 hours
  2. customThe mixture was evaporated to dryness in vacuo and water (500 ml)
  3. additionadded to the residue
  4. additionSodium hydroxide was added
  5. temperatureto raise the pH to ca. 5
  6. customThe solid which formed
  7. filtrationwas filtered off
  8. customrecrystallised from ethanol