HRID39304

反应详情

EQUATION

反应方程式

HRID 39304 的结构方程式

PROCEDURE

实验过程

3,6-Dichloro-pyridazine (1 g, 6/5 mmol) was placed in a flask fitted with a water condenser and methylhydrazine (1.31 mL, 25 mmol) was added dropwise. An immediate exotherm was observed and methylhydrazine begins to reflux. When the reaction had subsided, the mixture was left for 16 hours, and the excess methylhydrazine was removed under reduced pressure. The cooled residue was stirred with aqueous sodium hydroxide solution (20 ml of 20%), and the resulting solution was extracted with ether (6×100 ml). The combined extracts were dried (K2CO3) and concentrated to give 427 mg of N-(6-Chloro-pyridazin-3-yl)-N-methyl-hydrazine.

WORKUP

后处理

  1. customfitted with a water condenser
  2. temperatureto reflux
  3. customthe excess methylhydrazine was removed under reduced pressure
  4. extractionthe resulting solution was extracted with ether (6×100 ml)
  5. dry with materialThe combined extracts were dried (K2CO3)
  6. concentrationconcentrated