Ammonia → HCID 85549673, compound
Reaction equation
[F:1][CH:2]([C:8](=O)[C:9]([F:12])([F:11])[F:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[NH3:14]>C1(C)C=CC=CC=1>[NH2:14][C:8]([C:9]([F:12])([F:11])[F:10])=[C:2]([F:1])[C:3]([O:5][CH2:6][CH3:7])=[O:4]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Ethyl 2,4,4,4-tetrafluoro-3-oxobutanoate (81 g.) in toluene (60 ml) was stirred and heated to 70° C. whereupon ammonia gas was bubbled in until an uptake of 6.8 g. was recorded. The reaction was then set for reflux and water removed azeotropically. Approximately 10 ml of water was removed. After cooling, the solvent was removed under reduced pressure and the residue distilled to give ethyl 3-amino-2,4,4,4-tetrafluoro-2-butenoate b.p. 79°-86° C./20 mm, 44 g.
Workup
- customwas bubbled in until an uptake of 6.8 g
- temperaturefor reflux
- customwater removed azeotropically
- customApproximately 10 ml of water was removed
- temperatureAfter cooling
- customthe solvent was removed under reduced pressure
- distillationthe residue distilled
Sources & evidence
- ORD record
- ord-1c52539500b645c182927bb0d6e9964f
- Source dataset
- uspto-grants-1992_07
- Patent number
- US05134145
Reaction notes
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