참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethyl phosphite | HCID 31215 | — |
| 반응물 | 4-(4-Methoxybenzoyl)benzyl bromide | HCID 13150670 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Diethyl 4-(4-methoxybenzoyl)benzylphosphonate | HCID 89462655 | 72% |
반응 단계
(4-(bromomethyl)phenyl)(4-methoxyphenyl)methanone, 32-c, (3 g, 10 mmol) and triethyl phosphite (2 g, 11.9 mmol) was dissolved in DMF (20 ml), and then stirred for 10 h at 150° C. The resulting mixture was cooled to ambient temperature, diluted with water (50 ml) and extracted with ethyl acetate (3×50 ml). The organic layer was combined, washed with brine (2×100 ml), dried over Na2SO4 anhydrous, purified by chromatography on silica gel (petroleum ether/ethyl acetate=1:1.5). The pure product, 32-d, was obtained as a colorless oil (2.6 g, 72% yield). 1H NMR (300 MHz, CDCl3) δ 1.20-1.27 (m, 6H), 2.80-2.88 (d, J=22.8, 2H) 3.81 (s, 3H), 3.93-4.07 (m, 4H), 6.86-6.90 (m, 2H), 7.31-7.35 (m, 2H), 7.62-7.93 (m, 4H). LC-MS 363 [MH]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09079930B2 |
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| 출처 데이터셋 | uspto-grants-2015_07 |
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| ORD ID | ord-17276aeb6b5542bf8bbbcebcf41e85bf |
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| 출처 메모 | uspto-grants-2015_07 |
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