Hydrochloric Acid → 1-(2,6-Difluorophenyl)methanamine--hydrogen chloride (1/1)
Reaction equation
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[C:4]#[N:5].[ClH:11].[H][H]>O.C(O)C>[ClH:11].[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[CH2:4][NH2:5]Participants
6
Procedure
A mixture of 5.00 g. of 2,6-difluorobenzonitrile and 1.0 g. of 50% water-wet 5% palladium on carbon catalyst in 100 ml. of concentrated HCl and 100 ml. of absolute ethanol is shaken at room temperature under 20 lbs. pressure of hydrogen for 48 hours. The mixture is filtered and the filtrate is diluted with 500 ml. of diethyl ether and allowed to stand. Filtration gives the desired product as colorless crystals, m.p. 197°-200° C.
Workup
- additionA mixture of 5.00 g
- filtrationThe mixture is filtered
- additionthe filtrate is diluted with 500 ml
- filtrationFiltration
Sources & evidence
- ORD record
- ord-86ecba610cd448b1be5df9d91fb236ae
- Source dataset
- uspto-grants-1978_08
- Patent number
- US04107326
Reaction notes
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