참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Ethenyl-4-nitrobenzene | HCID 7481 | — |
| 반응물 | Trimethyl orthoformate | HCID 9005 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Phosphinic Acid | HCID 4124402 | — |
| 반응물 | HCID 178502919 | HCID 178502919 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178502925 | HCID 178502925 | — |
반응 단계
0.665 g of crystalline hypophosphorous acid was treated under nitrogen with 1.73 g of trimethyl orthoformate and the mixture was stirred at 20° C. for 2 hours. The resulting solution of crude methyl hypophosphite was added dropwise at 0° C. to a solution of 1 g of 4-nitrostyrene and 0.43 g of diisopropylethylamine in 5 ml of methanol. After 65 hours at 20° C. the same amount of methyl hypophosphite was again added and the mixture was stirred at 20° C. for a further 24 hours. The mixture was diluted with 30 ml of water and the pH was adjusted to 7 with aqueous sodium bicarbonate solution. After extraction with dichloromethane and chromatography on silica gel using 10% methanol in ethyl acetate for the elution there was obtained 0.5 g of 1-[2-(methoxyphosphinyl)ethyl]-4-nitrobenzene in the form of a yellow liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04743687 |
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| 출처 데이터셋 | uspto-grants-1988_05 |
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| ORD ID | ord-f4c21074e7fa4b37a69f58637e826285 |
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| 출처 메모 | uspto-grants-1988_05 |
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