Methylhydrazine → 3-Chloro-6-(1-methylhydrazinyl)pyridazine

3,6-Dichloro-pyridazine (1 g, 6.75 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.

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

ORD record

ord-930b54c604144b87ae5a3cc08574b5fa

Source dataset

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08884030B2