1-Diphenylmethylamino-2-phenylethylphosphonous acid → 1-Amino-2-phenylethylphosponous acid
Reaction equation
C1(C([NH:14][CH:15]([P:23]([OH: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>Br>[NH2:14][CH:15]([P:23]([OH:25])[OH:24])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
9.9 g (0.028 mol) of 1-diphenylmethylamino-2-phenylethylphosphonous acid are heated, at 100°-105° C. for 2 h, in 50 ml of 40% hydrobromic acid. The reaction solution is then evaporated to dryness i.V. and the residue is taken up in 50 ml of water. The aqueous solution is washed several times with diethyl ether and evaporated to dryness. The residue is dissolved in 60 ml of ethanol and propylene oxide is added to the solution until the product precipitates out. After the mixture has been left to stand overnight, the precipitate is filtered off with suction, washed with ethanol/diethyl ether and dried.
Workup
- customThe reaction solution is then evaporated to dryness i.V
- washThe aqueous solution is washed several times with diethyl ether
- customevaporated to dryness
- dissolutionThe residue is dissolved in 60 ml of ethanol
- additionpropylene oxide is added to the solution until the product
- customprecipitates out
- waitAfter the mixture has been left
- filtrationthe precipitate is filtered off with suction
- washwashed with ethanol/diethyl ether
- customdried
Sources & evidence
- ORD record
- ord-9aa50f4c9c224ff5aefb63bcf3db20c3
- Source dataset
- uspto-grants-1997_09
- Patent number
- US05663139
Reaction notes
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