Hydrochloric Acid → HCID 20556522, compound

HRID 1660101Notes

Reaction equation

HRID 1660101 reaction equation
[NH2:1][C:2]([P:9]([OH:12])(=[O:11])[OH:10])([P:5]([OH:8])(=[O:7])[OH:6])[CH2:3][CH3:4].[OH-].[Na+].[C:15]([OH:20])(=[O:19])/[CH:16]=[CH:17]/[CH3:18].Cl>O>[C:15]([CH:16]([NH:1][C:2]([P:5]([OH:8])(=[O:6])[OH:7])([P:9]([OH:12])(=[O:10])[OH:11])[CH2:3][CH3:4])[CH2:17][CH3:18])([OH:20])=[O:19]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2×HCID 637090Crotonic AcidHCID 436880715049-86-2

Product 1

HCID 20556522HCID 20556522, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
100 °C

Procedure

54.8 g. of 1-amino propane-1,1-diphosphonic acid and 40 g. of sodium hydroxide are dissolved in 150 cc. of water. 10 g. of sodium hydroxide dissolved in 40 cc. of water and 22 g. of crotonic acid dissolved in 50 cc. of water are added drop by drop simultaneously thereto while stirring vigorously. After continuing stirring for one hour, the temperature of the reaction mixture is increased to 100° C. and the reaction solution is boiled under reflux for 3 hours. It is then slightly acidified with hydrochloric acid. Any turbidity occurring thereby is removed by filtration. After treating the solution with an acid ion exchange agent, the N-(1-carboxy propyl)-1-amino propane-1,1-diphosphonic acid is obtained as an oily residue. This residue is mixed with 100 cc. of ethanol, the ethanol is decanted, and the residue is dried.

Workup

  1. stirringAfter continuing stirring for one hour
  2. temperatureunder reflux for 3 hours
  3. customAny turbidity occurring thereby is removed by filtration
  4. additionAfter treating the solution with an acid ion exchange agent

Sources & evidence

ORD record
ord-65bfc9403edf4b0dada449dc85d3c801
Source dataset
uspto-grants-1981_12
Patent number
US04307038

Reaction notes

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