HRID372636

反应详情

EQUATION

反应方程式

HRID 372636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of 6.3 grams of 2,4,6-trichloro-5-pyrimidinecarbonitrile in 25 ml of acetone was cooled to -10°, and 2.5 grams of 2-amino-2-methylpropionitrile was added. With the reaction mixture at -10°, a solution of 1.3 grams of sodium hydroxide in 3.5 ml of water was added dropwise. Upon complete addition, the reaction mixture was stirred at -10° for 30 minutes. The acetone was removed under reduced pressure; the residue was extracted with diethyl ether, and the extract was separated and dried over magnesium sulfate. The extract was filtered, and the filtrate was evaporated under reduced pressure, yielding a residue. The residue was recrystallized from methylcyclohexane to give 3.1 grams of 4,6-dichloro-2-(1-cyano-1-methylethylamino)-5-pyrimidinecarbonitrile; mp, 154-158°.

WORKUP

后处理

  1. additionUpon complete addition
  2. customThe acetone was removed under reduced pressure
  3. extractionthe residue was extracted with diethyl ether
  4. customthe extract was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe extract was filtered
  7. customthe filtrate was evaporated under reduced pressure
  8. customyielding a residue
  9. customThe residue was recrystallized from methylcyclohexane