Hydrazine hydrate (1:1) → 1154030-52-0
Reaction equation
Br[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([CH3:9])=[CH:4][N:3]=1.O.[NH2:11][NH2:12]>C(O)C>[NH:11]([C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([CH3:9])=[CH:4][N:3]=1)[NH2:12]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
3.8 g (18.4 mmol, purity 90%) of the compound from Example 20A are initially charged in 12.5 ml of ethanol. 8.9 ml (9.2 g, 183.8 mmol) of hydrazine hydrate are added, and the mixture is reacted in a single-mode microwave oven (CEM Explorer) at 170° C. (100 Watt) for 2 h. The reaction solution is then concentrated, and the residue is taken up in ethyl acetate and washed in each case once with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure.
Workup
- customthe mixture is reacted in a single-mode microwave oven (CEM Explorer) at 170° C. (100 Watt) for 2 h
- concentrationThe reaction solution is then concentrated
- washwashed in each case once with saturated sodium bicarbonate solution and saturated sodium chloride solution
- dry with materialThe organic phase is dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
Sources & evidence
- ORD record
- ord-7535d233287e4b47817e13f3bf7c4463
- Source dataset
- uspto-grants-2013_12
- Patent number
- US08609698B2
Reaction notes
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