Hydrogen Peroxide → Glycidylphosphonic acid dimethyl ester

HRID 437046

반응식

HRID 437046 반응식
[CH3:1][O:2][P:3]([CH2:7][CH:8]=[CH2:9])(=[O:6])[O:4][CH3:5].[OH:10]O>CC(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.[V]>[CH3:1][O:2][P:3]([CH2:7][CH:8]1[O:10][CH2:9]1)(=[O:6])[O:4][CH3:5]

참가 물질

5

반응물 2

HCID 784Hydrogen PeroxideHCID 136570Dimethyl allylphosphonate

생성물 1

HCID 298005Glycidylphosphonic acid dimethyl ester

시약·촉매·용매 2

HCID 5377225Vanadium(III) acetylacetonate촉매HCID 180Acetone용매

실험 절차

In a flask having a capacity of 500 ml, equipped with a stirrer, thermostatic temperature control, reflux condenser, dropping funnel and internal thermometer, 0.5 g of vanadium (III) acetylacetonate is dissolved in 120 ml of acetone (previously purified with KMnO4). Then 75 g (0.5 mole) of allylphosphonic acid dimethyl ester is mixed in. With intense stirring, 65 ml of 30% hydrogen peroxide is added drop by drop over a period of about 20 minutes at 30° C. Then the mixture is refluxed for 2 hours, after which the acetone is largely removed by distillation, whereupon the product separates as the heavy phase. The aqueous phase is extracted with methylene chloride. 77 grams of glycidylphosphonic acid dimethyl ester are obtained by vacuum distillation.

후처리

  1. customIn a flask having
  2. customa capacity of 500 ml, equipped with a stirrer
  3. temperaturethermostatic temperature control, reflux condenser
  4. custompreviously purified with KMnO4)
  5. temperatureThen the mixture is refluxed for 2 hours
  6. customafter which the acetone is largely removed by distillation, whereupon the product
  7. extractionThe aqueous phase is extracted with methylene chloride

출처 및 근거

ORD 기록
ord-b4d437c0a3544b4189d2ed4ba386f02c
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04029679

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