참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Oxygen | HCID 977 | — |
| 반응물 | 2,3-Dihydro-1-methyl-1H-phosphole 1-oxide | HCID 70104 | — |
| 반응물 | Methane phosphonous acid methyl ester | HCID 54069057 | — |
| 생성물 | 1-Methyl-1-oxophospholanyl methyl phosphinic acid methyl ester | HCID 53880998 | 277.5% |
반응 단계
6 g of tert.-butyl peroctoate in 30 g of methane phosphonous acid methyl ester and 116 g of 1-methyl-1-oxophospholine are added dropwise to 282 g of oxygen-free methane phosphonous acid methyl ester at 120° C. with stirring. The reaction time is 90 minutes. Excess methane phosphonous acid methyl ester and a small quantity of 1-methyl-oxophospholine are distilled off. The residue, consisting of 205 g of 1-methyl-1-oxophospholanyl-methyl phosphinic acid methyl ester is purified by distillation under vacuum (bp1 mm : 210° to 220° C.) to yield 186 g of pure product which solidifies very slowly to stellate crystals which begin to reliquefy at 70° C. Acid saponification leads to isomeric 1-methyl-1-oxophospholanylmethyl phosphinic acids of the idealized constitution: ##STR17##
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04294719 |
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| 출처 데이터셋 | uspto-grants-1981_10 |
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| ORD ID | ord-3a0b11b509fc43e882b4cf004b5b9e93 |
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| 출처 메모 | uspto-grants-1981_10 |
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