HRID598080

反应详情

EQUATION

反应方程式

HRID 598080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

A mixture of 12.8 g (99.9 mmol) of 2-thiouracil and 4.3 g (108 mmol) of sodium hydroxide was placed in 500 ml Erlenmeyer flask, and dissolved on the oil bath with a minimum amount of water. Twice the volume of 99% ethanol was then added, the solution cooled to 30° C., and 6.3 ml (99.9 mmol) of methyl iodide added. The solution was heated to 60° C. for 20 min, then cooled to room temp. The precipitate was filtered off, and, after acidifying the filtrate with acetic acid, the excess solvent was removed in vacuo. The combined precipitates were thoroughly washed with water and recrystallized from ethanol to give 6.0 g (47%) of product.

WORKUP

后处理

  1. temperatureThe solution was heated to 60° C. for 20 min
  2. temperaturecooled to room temp
  3. filtrationThe precipitate was filtered off
  4. customthe excess solvent was removed in vacuo
  5. customThe combined precipitates
  6. washwere thoroughly washed with water
  7. customrecrystallized from ethanol