Potassium Carbonate → HCID 53686113, compound

HRID 1198774Notes

Reaction equation

HRID 1198774 reaction equation
[CH2:1]([O:3][P:4]([CH:9]([NH2:18])[P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[O:19]([CH2:26][CH2:27][CH2:28]Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[CH2:12]([O:11][P:10]([CH:9]([NH:18][CH2:28][CH2:27][CH2:26][O:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[P:4]([O:5][CH2:6][CH3:7])(=[O:8])[O:3][CH2:1][CH3:2])(=[O:17])[O:14][CH2:15][CH3:16])[CH3:13]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 68522Benzene, (3-bromopropoxy)-HCID 2773808Tetraethyl aminomethylenediphosphonate

Product 1

HCID 53686113HCID 53686113, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

3.03 g (0.01 mol) of aminomethylenediphosphonic acid tetraethyl ester, 2.3 g (0.01 mol) of 3-phenoxypropylbromide and 1.4 g (0.01 mol) of potassium carbonate are dissolved in 50 ml of dioxane and stirred under reflux for 24 hours. The major part of the solvent is distilled off, and the residue is partitioned between water and ethyl acetate. The organic layer is separated, washed with water, dried over sodium sulphate and evaporated to dryness yielding raw N-(3-phenoxypropyl)aminomethanediphosphonic acid tetraethyl ester which may be used without further purification.

Workup

  1. temperatureunder reflux for 24 hours
  2. distillationThe major part of the solvent is distilled off
  3. customthe residue is partitioned between water and ethyl acetate
  4. customThe organic layer is separated
  5. washwashed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness

Sources & evidence

ORD record
ord-9526731772464338a01689b855faf002
Source dataset
uspto-grants-1994_01
Patent number
US05281748

Reaction notes

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