Hydrochloric Acid → Ethyldiethylaminomethylphosphinic acid

HRID 923818Notes

Reaction equation

HRID 923818 reaction equation
[CH2:1]=O.Cl.[CH2:4]([NH:6][CH2:7][CH3:8])[CH3:5].[CH2:9]([P:11]([OH:13])[OH:12])[CH3:10].Cl>O>[CH2:9]([P:11]([CH2:1][N:6]([CH2:7][CH3:8])[CH2:4][CH3:5])(=[O:13])[OH:12])[CH3:10]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10197650Diethylammonium chlorideHCID 13411864Ethylphosphonous acid

Product 1

HCID 46843572Ethyldiethylaminomethylphosphinic acid

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A three-neck round-bottom flask with fitted KPG stirrer, reflux condenser and dropping funnel is initially charged with 44.0 g of paraformaldehyde (95%), 105.5 g of demineralized water and 233.4 g of diethylamine hydrochloride, followed by the addition of 100.1 g of ethylphosphonous acid (96.3%) (prepared according to example 1) during 6 h at 110° C. with stirring. The pH of the reaction solution is adjusted to below 1 with 8 g of 37% hydrochloric acid. After one hour of refluxing, a solution of ethyldiethylaminomethylphosphinic acid is obtained.

Workup

  1. temperatureA three-neck round-bottom flask with fitted KPG stirrer, reflux condenser
  2. temperatureAfter one hour of refluxing

Sources & evidence

ORD record
ord-86819919d05a4de3b3277b3857e66e9b
Source dataset
uspto-grants-2016_03
Patent number
US09279085B2

Reaction notes

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