Water → HCID 14976000, compound
Reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH:7]([OH:16])[C:8]([F:15])([F:14])[C:9](OCC)=[O:10].O.[NH2:18][NH2:19].O>CCO>[F:14][C:8]([F:15])([CH:7]([OH:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1)[C:9]([NH:18][NH2:19])=[O:10]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To stirring solution of 0.96 g (4.1 mmol) of ethyl 3-(2-pyridyl)-3-hydroxy-2,2-difluoropropanoate, prepared as described by Hallinan and Fried, Tetrahedron Lett., 25, 2301 (1984), in 8 mL of EtOH was added 0.41 g (8.2 mmol) of hydrazine hydrate. After 16 hours, a yellow precipitate had formed. To the reaction was added H2O. The precipitate was filtered and washed with a minimum of H2O. The yield of product was 0.44 g (49%) after drying in a steam cabinet. Analysis calculated for C8H9N3O2F2 (M.W. 217.18): C, 44.24; H, 4.18; N, 19.35. Found: C, 44.07; H, 4.16; N, 19.05.
Workup
- customprepared
- customa yellow precipitate had formed
- filtrationThe precipitate was filtered
- washwashed with a minimum of H2O
- customafter drying in a steam cabinet
Sources & evidence
- ORD record
- ord-afb83527bba14d809570ccfd3fa32859
- Source dataset
- uspto-grants-1995_11
- Patent number
- US05464830
Reaction notes
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