참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | Dimethyl allylphosphonate | HCID 136570 | — |
| 촉매 | Vanadium(III) acetylacetonate | HCID 5377225 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | Glycidylphosphonic acid dimethyl ester | HCID 298005 | — |
반응 단계
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 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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04048374 |
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| 출처 데이터셋 | uspto-grants-1977_09 |
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| ORD ID | ord-80e5cd0459cc4c6b8f3a5e13ba7979e6 |
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| 출처 메모 | uspto-grants-1977_09 |
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