Methylhydrazine → HCID 57280465, compound
Reaction equation
[OH:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[OH:13])[C:5](OCC)=[O:6].[CH3:14][NH:15][NH2:16]>>[CH3:14][N:15]([C:5](=[O:6])[C:4]1[CH:10]=[CH:11][C:12]([OH:13])=[C:2]([OH:1])[CH:3]=1)[NH2:16]Participants
3
Procedure
0.11 g (0.05 mol) of 3,4-dihydroxybenzoic acid, ethyl ester and 106 ml of methylhydrazine (2 mol) were refluxed for 3 days. The reaction mixture was evaporated in vacuo and the oily residue treated with ethanol and evaporated again. This was repeated once more. After retreatment with ethanol, 3,4-dihydroxybenzoic acid, 1-methylhydrazide began to crystallize. The crude product was removed by filtration and recrystallized from ethanol; yield: 3.8 g, melting point 202°-205° C.
Workup
- customThe reaction mixture was evaporated in vacuo
- additionthe oily residue treated with ethanol
- customevaporated again
- customto crystallize
- customThe crude product was removed by filtration
- customrecrystallized from ethanol
Sources & evidence
- ORD record
- ord-c5299031cebb41229891fe775c6129c3
- Source dataset
- uspto-grants-1989_01
- Patent number
- US04801705
Reaction notes
Loading…