Ammonium Hydroxide → Fosamine ammonium

HRID 328289

Reaction equation

HRID 328289 reaction equation
[OH-].[NH4+:2].[C:3]([P:7](=[O:14])([O:11]CC)[O:8][CH2:9][CH3:10])(OC)=[O:4]>>[C:3]([P:7](=[O:14])([O-:11])[O:8][CH2:9][CH3:10])(=[O:4])[NH2:2].[NH4+:2]

Participants

3

Reactant 2

HCID 14923Ammonium HydroxideHCID 170573Phosphinecarboxylic acid, diethoxy-, methyl ester, oxide

Product 1

HCID 33256Fosamine ammonium

Conditions

Temperature
15 °C

Procedure

A solution of 48.5 parts of 29% aqueous ammonium hydroxide is stirred and cooled with an external ice bath to 15° C. To the cooled solution 20.5 parts of diethyl carbomethoxyphosphonate is slowly added over a 10 minute period. The mixture turns cloudy, but clears up after about 15 minutes. During this time, the mixture is allowed to warm spontaneously to about 30° C. and stirring is continued for 2 hours. The clear solution is stripped under reduced pressure (15 mm of Hg) at a water-bath temperature of 70° C. The residue is a white crystalline solid which is recrystallized from absolute ethyl alcohol, giving 11.7 parts of ammonium ethyl carbamoylphosphonate, m.m. 173°-176° C.

Workup

  1. temperatureto warm spontaneously to about 30° C.
  2. waitis continued for 2 hours
  3. customThe clear solution is stripped under reduced pressure (15 mm of Hg) at a water-bath
  4. customtemperature of 70° C
  5. customis recrystallized from absolute ethyl alcohol

Sources & evidence

ORD record
ord-82405dbbb1f24a7e963f6d4140535fa2
Source dataset
uspto-grants-1977_04
Patent number
US04017296

Linked notes

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