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

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.

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レコード

ord-facf30b996f1484aaf341a84a6141e83

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524764B2