Phosphinic acid, bis(1,1-dimethylethyl)- synthesis

7synthesis methods

Product Name:Phosphinic acid, bis(1,1-dimethylethyl)-
CAS Number:677-76-9
Molecular formula:C8H19O2P
Molecular Weight:178.209

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Phosphinic acid, bis(1,1-dimethylethyl)-

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Yield:-

Reaction Conditions:

Stage #1: acetic acid tert-butyl esterwith sodium hypophosphite;2,2'-azobis(isobutyronitrile);sulfuric acid;acetic acid at 60; under 750.075 Torr; for 6 h;
Stage #2: with di-tert-butyl peroxide at 110; under 3000.3 Torr; for 8 h;Reagent/catalyst;Pressure;Temperature;

Steps:

3 Example 3 Synthesis of diisobutyl phosphonic acid:

(1) in the reactor by 1: 1 ratio of acetic acid and sodium hypophosphite, stirring enough to dissolve, stirring speed in the60r / min, adding sulfuric acid to react, the molar ratio of sodium hypophosphite to sulfuric acid is 2: 1, the reaction time is 1 hour, the temperature rises to50 ° C.(2) followed by addition of t-butyl acetate in an equal proportion to acetic acid and 2% by weight of azobisisobutyronitrileAfter dissolving, a macroporous strong acid cation exchange resin containing 1% by weight of tert-butyl ester was added, stirring was continued, the temperature was raised, the temperature was maintained at 60C,And maintain the pressure to maintain within 0.1MPa.(3) After 6 hours of reaction,Again, 2% by weight of tert-Of di-tert-butyl peroxyAnd the remaining tert-butyl esterThe mass ratio of tert-butyl ester to acetic acid was 1.25,And added to the tert-butyl ester2 wt%Of the activator polyethylene glycol at 0.025 ° C / minHeating rate of heating to 110 , the pressure maintained at 0.4MPa, stirring speed 30r / min, holding temperature for 8 hours, insulation junctionAfter the reaction, the reaction vessel is naturally cooled to obtain the product.

References:

CN106518915,2017,A Location in patent:Paragraph 0032; 0033; 0034; 0035; 0036; 0037; 0038-0047