Methylhydrazine → HCID 86707218, compound
Reaction equation
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9](=O)[CH:10]=[CH:11][N:12](C)[CH3:13])=[C:4]([F:16])[CH:3]=1.C[NH:18]N>CO>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH:10]=[CH:11][N:12]([CH3:13])[N:18]=2)=[C:4]([F:16])[CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 1-(4-bromo-2,6-difluorophenyl)-3-(dimethylamino)-2-propene-1-one (i.e. the product of Step A, 2.39 g, 8.24 mmol) and methylhydrazine (0.42 g, 9.05 mmol) in methanol (50 mL) was stirred at room temperature overnight. The reaction mixture was then concentrated under reduced pressure, and the residue was purified by medium pressure liquid chromatography on silica gel eluted with 0 to 100% ethyl acetate in hexanes to yield the title compound (0.86 g).
Workup
- concentrationThe reaction mixture was then concentrated under reduced pressure
- customthe residue was purified by medium pressure liquid chromatography on silica gel
- washeluted with 0 to 100% ethyl acetate in hexanes
Sources & evidence
- ORD record
- ord-97edef35f0e34ee9ba9b3fb1f5f44504
- Source dataset
- uspto-grants-2014_08
- Patent number
- US08815772B2
Reaction notes
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