Hydrogen Bromide → HCID 178419704, compound
Reaction equation
C1(C([NH:14][CH:15]([PH:23](=[O:25])[OH:24])[CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)C2C=CC=CC=2)C=CC=CC=1.[BrH:26]>>[BrH:26].[NH2:14][CH:15]([PH:23](=[O:24])[OH:25])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1Participants
3
Procedure
A mixture of 14.6 g (41.6 mmol) of [1-[(diphenylmethyl)amino]-2-phenylethyl]phosphinic acid and 94 ml of aqueous 48% hydrobromic acid is refluxed for 2 hours. Two phases appear. The mixture is brought to dryness by evaporation under vacuum and under warm conditions and is then taken up in 94 ml of water. The aqueous phase is washed three times with diethyl ether. The aqueous phase, again evaporated, gives (1-amino-2-phenylethyl)phosphinic acid hydrobromide, which is taken up in 58 ml of absolute ethanol. 20.4 ml of propylene oxide are added dropwise, with stirring, at 0° C. The formation of an abundant white precipitate is observed, which is filtered off and washed with diethyl ether. 6.77 g of product are recovered (yield=87.9%).
Workup
- temperatureis refluxed for 2 hours
- customThe mixture is brought to dryness by evaporation under vacuum and under warm conditions
- washThe aqueous phase is washed three times with diethyl ether
- customThe aqueous phase, again evaporated
Sources & evidence
- ORD record
- ord-d4968668cc974f3fbbe46a3a2c475269
- Source dataset
- uspto-grants-2003_02
- Patent number
- US06518260B1
Reaction notes
Loading…