Azobisisobutyronitrile → HCID 46901656, compound

HRID 1914965Notes

Reaction equation

HRID 1914965 reaction equation
[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[CH3:6][C:7](=[CH2:10])[CH2:8][OH:9].CC(N=NC(C#N)(C)C)(C#N)C>C(O)(=O)C>[CH2:1]([P:3]([CH2:6][CH:7]([CH3:10])[CH2:8][OH:9])(=[O:5])[OH:4])[CH3:2]

Participants

5

Reactant 3

HCID 6547AzobisisobutyronitrileHCID 10557Methallyl alcoholHCID 13411864Ethylphosphonous acid

Product 1

HCID 46901656HCID 46901656, compoundYield 92.1%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent2×

Procedure

94 g (1 mol) of ethylphosphonous acid (produced as in Example 1) and 114 g (1 mol) of 2-methyl-2-propen-1-ol are initially charged in 200 ml of glacial acetic acid in a four-neck round-bottom flask equipped with stirrer, reflux condenser, thermometer and nitrogen inlet and heated. At about 100° C., 98.4 g of a 5% solution of AIBN in glacial acetic acid are added dropwise over 1 h. Thereafter, the solvent was distilled off in vacuo to leave 153 g of ethyl(2-methyl-3-hydroxypropyl)phosphinic acid.

Workup

  1. customequipped with stirrer
  2. temperaturereflux condenser
  3. temperaturethermometer and nitrogen inlet and heated
  4. distillationThereafter, the solvent was distilled off in vacuo

Sources & evidence

ORD record
ord-2454d299b92f4366a20b44f135d6a936
Source dataset
uspto-grants-2013_12
Patent number
US08614267B2

Reaction notes

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