HRID2247849

反应详情

EQUATION

反应方程式

HRID 2247849 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture containing 0.71 g (5 mmol) of 6-methyl-2-thiouracil, 0.76 g (5 mmol) of 2-dimethylaminobenzyl alcohol (J. Chem. Soc. 1954, 4127) and 5 ml of concentrated hydrochloric acid is stirred at 60° C. for 3 hours, then cooled and made alkaline by adding 5N sodium hydroxide solution under cooling by ice. The mixture is extracted 3 times with 20 ml of chloroform each. After combining the organic phase is washed with sodium carbonate solution and then with saturated sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated. The residue is twice recrystallized from ethyl acetate to yield 0.59 g (43%) of the title compound, m.p.: 151°-153° C.

WORKUP

后处理

  1. temperaturecooled
  2. temperatureunder cooling by ice
  3. extractionThe mixture is extracted 3 times with 20 ml of chloroform each
  4. washis washed with sodium carbonate solution
  5. dry with materialwith saturated sodium chloride solution, dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe residue is twice recrystallized from ethyl acetate