Ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate → 3-Amino-2-methylpropylphosphonous acid monohydrate
Reaction equation
[NH2:1][CH2:2][CH:3]([CH3:17])[CH2:4][P:5](C(OCC)OCC)(=[O:9])[O:6]CC>Cl>[OH2:6].[NH2:1][CH2:2][CH:3]([CH3:17])[CH2:4][P:5]([OH:9])[OH:6]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 6.0 g of ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate in 30 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 7 hours. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure and co-evaporated twice with 10 ml water under reduced pressure and co-evaporated twice with 10 ml of water under reduced pressure. The crude product is dissolved in 50 ml of dry ethanol and 5 ml of propylene oxide is added dropwise. The precipitated solid is collected by filtration and dried to give 3-amino-2-methylpropylphosphonous acid monohydrate, m.p. 96°-100° C., 31P=+25.8 ppm (D2O).
Workup
- temperatureto reflux for a period of 7 hours
- concentrationconcentrated under reduced pressure
- dissolutionThe crude product is dissolved in 50 ml of dry ethanol
- addition5 ml of propylene oxide is added dropwise
- filtrationThe precipitated solid is collected by filtration
- customdried
Sources & evidence
- ORD record
- ord-568ded0d150d452da6c7c01ba637ea25
- Source dataset
- uspto-grants-1988_09
- Patent number
- US04772738
Reaction notes
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