HRID1291219

反应详情

EQUATION

反应方程式

HRID 1291219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In ethanol-water (2:1) (45 ml)was dissolved 2-t-butyl-4,5-dichloro-3(2H)-pyridazinone (4.4 g) followed by addition of 50% dimethylamine (7.2 g), and the mixture was stirred at room temperature for 15 hours. After removal of ethanol, the residue was extracted with diethyl ether and the organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. This residue was washed with n-hexane and dried. White powder, 4.4 g. 1H-NMR (CDCl3) δ: 1.63(9H,s), 3.10(6H,s), 7.57(1H,s).

WORKUP

后处理

  1. customAfter removal of ethanol
  2. extractionthe residue was extracted with diethyl ether
  3. washthe organic layer was washed with saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated to dryness
  6. washThis residue was washed with n-hexane
  7. customdried