Hydrochloric Acid → HCID 10154248, compound
Reaction equation
[NH2:1][CH2:2][CH2:3][CH2:4][P:5]([CH:10]([F:12])[F:11])(=[O:9])[O:6]CC.Cl>>[NH2:1][CH2:2][CH2:3][CH2:4][P:5]([CH:10]([F:12])[F:11])(=[O:6])[OH:9]Participants
3
Procedure
A mixture of 520 mg (2.6 mmol) of ethyl P-(3-aminopropyl)-P-difluoromethyl-phosphinate and 5 ml of 12M hydrochloric acid is refluxed for 3 hours and then evaporated to dryness. The residue is dissolved in 5 ml of methanol. To the stirred solution 25 ml of epoxypropane are added dropwise, upon which spontaneous crystallisation occurs. The crystals are collected and dried yielding P-(3-aminopropyl)-P-difluoromethyl-phosphinic acid of m.p. 261°.
Workup
- temperatureis refluxed for 3 hours
- customevaporated to dryness
- dissolutionThe residue is dissolved in 5 ml of methanol
- additionTo the stirred solution 25 ml of epoxypropane are added dropwise, upon which spontaneous crystallisation
- customThe crystals are collected
- customdried
Sources & evidence
- ORD record
- ord-c2911a0eb28b4d939ebe7a5c2134bf85
- Source dataset
- uspto-grants-1994_01
- Patent number
- US05281747
Reaction notes
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