Ammonium Chloride → HCID 86744061, compound

HRID 2165048Notes

Reaction equation

HRID 2165048 reaction equation
C([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH:13]([P:20]([OH:23])(=[O:22])[OH:21])[CH:14]([OH:19])[P:15]([OH:18])(=[O:17])[OH:16])C1C=CC=CC=1.[Na].[Cl-].[NH4+]>N>[NH:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH:13]([P:20]([OH:23])(=[O:21])[OH:22])[CH:14]([OH:19])[P:15]([OH:17])(=[O:16])[OH:18]

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 86744062HCID 86744062, compound

Product 1

HCID 86744061HCID 86744061, compound

Reagents, catalysts & solvents 1

HCID 222AmmoniaSolvent

Procedure

3.4 g (0.0094 mole) of 2-(1-benzylimidazol-2-yl)-1-hydroxyethanediphosphonic acid are dissolved in 40 ml of liquid ammonia and then 1 g of sodium is added gradually, with stirring, in small portions until the blue colour of the solution is maintained for some considerable time. Then 2.35 g of ammonium chloride are added in portions. The ammonia is then removed by evaporation, the residue is taken up in 20 ml of hot water, the solution is filtered and then 10 ml of concentrated hydrochloric acid are added to the filtrate. The precipitated crystals are isolated by filtration and recrystallised from aqueous methanol, to give 2-(imidazol-2-yl)-1-hydroxyethanediphosphonic acid of m.p. 235° C. (dec.).

Workup

  1. temperatureis maintained for some considerable time
  2. customThe ammonia is then removed by evaporation
  3. filtrationthe solution is filtered
  4. addition10 ml of concentrated hydrochloric acid are added to the filtrate
  5. customThe precipitated crystals are isolated by filtration
  6. customrecrystallised from aqueous methanol

Sources & evidence

ORD record
ord-4840222adbe040bb9ab8f063e050f1b8
Source dataset
uspto-grants-1990_07
Patent number
US04939130

Reaction notes

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