Hydrochloric Acid → HCID 11768978, compound

HRID 1683661Notes

Reaction equation

HRID 1683661 reaction equation
[CH2:1]([P:3]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:7])[O:4]CC)[CH3:2].Cl>C(O)C>[CH2:1]([P:3]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:4])[OH:7])[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 11008893ethyl ethylphenylphosphinate

Product 1

HCID 11768978HCID 11768978, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of ethyl (ethyl)(phenyl)phosphinate (130 mg, 0.66 mmol) in ethanol (0.5 ml) was treated with 4N HCl (1 ml) and refluxed for 22 hours. Tlc analysis revealed some residual starting material. The ethanol was removed on the rotary evaporator, an additional aliquot of 4N HCl (1 ml) was added, and reflux was resumed for a further six hours whereupon tlc analysis revealed complete consumption of starting material. The mixture was lyophillized to afford 110 mg (99%) of the title compound as a white solid; MS: 171 m/z (M+H)+ ; analysis calculated for C8H11O2P: C, 56.47; H, 6.53; P, 18.20; Found: C, 56.23; H, 6.35; P, 18.52.

Workup

  1. temperaturerefluxed for 22 hours
  2. customThe ethanol was removed on the rotary evaporator
  3. additionan additional aliquot of 4N HCl (1 ml) was added
  4. temperaturereflux
  5. customconsumption of starting material

Sources & evidence

ORD record
ord-c05243b7c41d45c5b0588eed618769d2
Source dataset
uspto-grants-1997_06
Patent number
US05639732

Reaction notes

Loading…