Sodium Hydroxide → HCID 86637085, compound

HRID 446630Notes

Reaction equation

HRID 446630 reaction equation
[C:1]([NH:5][CH2:6][P:7](=[O:10])([OH:9])[OH:8])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+:12]>CO>[C:1]([NH:5][CH2:6][P:7](=[O:8])([O-:10])[O-:9])([CH3:4])([CH3:3])[CH3:2].[Na+:12].[Na+:12]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 20512660HCID 20512660, compound

Product 1

HCID 86637085HCID 86637085, compoundYield 86.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

tert-Butylaminomethylphosphonic acid (18.4 g, 0.11 mol) was added to sodium hydroxide (8.8 g, 0.22 mol) solution in methanol (100 mL). The mixture was stirred under reflux for 2 hours. The mixture was concentrated in vacuum until solidifying (approximately to ⅓ of volume) and diethyl ether was added (200 mL). The precipitate was filtered and washed with diethyl ether to give disodium tert-butylaminomethylphosphonate (20 g, 86%), white micro-crystals, decomposition 350-400° C.; 1H NMR (D2O) δ 1.02 (s, 9H), 2.47 (d, J=15.0 Hz, 2H); 13C NMR δ 26.4, 40.1 (d, J=136.3 Hz), 50.6 (d, J=12.0 Hz).

Workup

  1. temperatureunder reflux for 2 hours
  2. concentrationThe mixture was concentrated in vacuum until solidifying (approximately
  3. additionwas added (200 mL)
  4. filtrationThe precipitate was filtered
  5. washwashed with diethyl ether

Sources & evidence

ORD record
ord-63302dd9062044d0bb1e2b41ea9f90c0
Source dataset
uspto-grants-2013_07
Patent number
US08480795B2

Reaction notes

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