Methylhydrazine → HCID 9903609, compound
Reaction equation
[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12](=O)[CH:13]([CH3:18])[CH2:14][C:15](O)=[O:16])=[CH:11][C:5]=2[O:4][CH2:3]1.[CH3:20][NH:21][NH2:22]>C(O)C>[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]3[CH:13]([CH3:18])[CH2:14][C:15](=[O:16])[N:21]([CH3:20])[N:22]=3)=[CH:11][C:5]=2[O:4][CH2:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
4-(3,4-Dihydro-3-oxo-1,4(2H)-benzoxazin-7-yl)-4-oxo-3-methylbutyric acid (1.56 g, 6.0 mmoles) was dissolved in ethanol (300 ml) and methylhydrazine (0.33 ml, 6.0 mmoles) was added. The mixture was heated at reflux for 2 hours, and then cooled to yield to yield the titled compound. The crystals were collected by filtration, recrystallized from ethanol, and recollected by filtration. The solid was dried under vacuum to yield 1.0 g of the titled compound, mp 204°-206° C.
Workup
- temperatureThe mixture was heated
- temperatureat reflux for 2 hours
- temperaturecooled
- customto yield
Sources & evidence
- ORD record
- ord-ab293ee570ac4156938e385ba76c9c40
- Source dataset
- uspto-grants-1993_06
- Patent number
- US05221742
Reaction notes
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