Methylhydrazine → 2-(1-Methylhydrazin-1-yl)pyrazine
Reaction equation
Cl[C:2]1[CH:7]=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:8][NH:9][NH2:10]>>[CH3:8][N:9]([C:2]1[CH:7]=[N:6][CH:5]=[CH:4][N:3]=1)[NH2:10]Participants
3
Procedure
2-Chloropyrazine (1 g, 8.3 mmol) and methylhydrazine (1.31 mL, 25 mmol) were mixed together in a flask fitted with a water condenser. After a few minutes an exotherm was observed. After 16 h 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 a light orange solid 370 mg of N-Methyl-N-pyrazin-2-yl-hydrazine.
Workup
- customfitted with a water condenser
- waitAfter a few minutes an exotherm was observed
- customAfter 16 h the excess methylhydrazine was removed under reduced pressure
- extractionthe resulting solution was extracted with ether (6×100 ml)
- dry with materialThe combined extracts were dried (K2CO3)
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-28a4d71b5ba24896aa0d31b613757e0e
- Source dataset
- uspto-grants-2013_09
- Patent number
- US08524764B2
Reaction notes
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