HRID372639

反应详情

EQUATION

反应方程式

HRID 372639 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 6.3 grams of 2,4,6-trichloro-5-pyrimidinecarbonitrile in 150 ml of diethyl ether was cooled to -10°, and a solution of 4.4 grams of diethylamine in 75 ml of diethyl ether was added dropwise. Upon complete addition, the reaction mixture was stirred at -10° for 1 hour. Water was added to the reaction mixture. The diethyl ether layer was separated and dried over magnesium sulfate. The mixture was filtered, and the filtrate was evaporated under reduced pressure to a residue. The residue was recrystallized from methylcyclohexane to give 3.8 grams of 4,6-dichloro-2-diethylamino-5-pyrimidinecarbonitrile; mp, 125°-126°.

WORKUP

后处理

  1. additionUpon complete addition
  2. customThe diethyl ether layer was separated
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe mixture was filtered
  5. customthe filtrate was evaporated under reduced pressure to a residue
  6. customThe residue was recrystallized from methylcyclohexane