HRID1862827

反应详情

EQUATION

反应方程式

HRID 1862827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

230 parts of 2,4,6-trichloro-5-methylthio-pyrimidine are dissolved in 740 parts of methylethylketone, 650 parts of ice are added, and 120 parts of an aqueous 38% solution of ethylamine are run in over 30 minutes while cooling in order that the temperature should not exceed 5° C. 129.5 parts of a 31% solution of caustic soda are added in a period of an hour at 20° C. and the mixture is stirred for 6 hours. The desired isomer is then precipitated while the 4-ethylamino-2,6-dichloro-5-methylthiopyrimidine remains in solution. After cooling for 15 hours, the product is filtered off and washed with methylethylketone. 73 parts of the desired product are obtained, which is recrystallised from ethanol. M.p. 147° C.

WORKUP

后处理

  1. additionare added
  2. customare run in over 30 minutes
  3. temperaturewhile cooling in order that the temperature should not
  4. customexceed 5° C
  5. customThe desired isomer is then precipitated while the 4-ethylamino-2,6-dichloro-5-methylthiopyrimidine
  6. temperatureAfter cooling for 15 hours
  7. filtrationthe product is filtered off
  8. washwashed with methylethylketone