Hydrogen Peroxide → Glycidylphosphonic acid dimethyl ester

HRID 437046

反応式

HRID 437046 の反応式
[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]

参加物

5

反応物 2

HCID 784Hydrogen PeroxideHCID 136570Dimethyl allylphosphonate

生成物 1

HCID 298005Glycidylphosphonic acid dimethyl ester

試薬・触媒・溶媒 2

HCID 5377225Vanadium(III) acetylacetonate触媒HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b4d437c0a3544b4189d2ed4ba386f02c
出典データセット
uspto-grants-1977_06
特許番号
US04029679

関連ノート

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