참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- | HCID 10036050 | — |
| 반응물 | 1-Iodo-5-(4-methoxyphenyl)-3-pentanone | HCID 13065019 | — |
| 반응물 | Nitro ketone | HCID 54223030 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3,4-Dimethoxyphenyl)-7-(4-methoxyphenyl)-2-nitro-5-heptanone | HCID 13065020 | — |
반응 단계
To a solution of 15 g. (0.071 mole) of 2-(3,4-dimethoxyphenyl)-1-nitroethane in 200 ml. of dry tetrahydrofuran was added 33.45 g. (0.08 mole) of 40% Triton B at room temperature. The solution was stirred at room temperature for 14 minutes under N2. 22.6 g. (0.071 mole) of 1-iodo-5-(4-methoxyphenyl)-3-pentanone was then added in portions. The mixture was heated at 50°-55° for 2 hours under N2 until no more starting material was detected on TLC, and then cooled to room temperature. The resulting reaction solution was poured into cold dil. HCl and extracted with ethyl acetate. The organic layer was dried over anhydrous MgSO4. The crude material was chromatographed on Florisil to provide 22 g. of desired nitro ketone derivative. Recrystallization from 80% ethanol gave a white solid which has m.p. 87°-89° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04342692 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-3f5f0db0de82463591055f422ac4d9a0 |
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| 출처 메모 | uspto-grants-1982_08 |
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