참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Malonic Acid | HCID 867 | — |
| 반응물 | Dibenzosuberol | HCID 14588 | — |
| 생성물 | 10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylacetic acid | HCID 12669091 | — |
반응 단계
A round-bottom flask, equipped with a distillation apparatus, is charged with dibenzosuberol (25.0 g, 0.119 mol) and malonic acid (61.9 g, 0.595 mol). The mixture is heated in an 160° C. oil bath. The solids melt. Gas bubbles form and water and acetic acid are distilled through the condenser. After 30 minutes, the mixture is cooled to room temperature and dissolved in ethyl acetate. The organic solution is washed with brine and dried (magnesium sulfate). The solvent is removed in vacuo to give an off white solid, which is recrystallized from hexane-ethyl acetate/1:1 to yield the title compound as white crystals, 28.8 g; mp 164°-165° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05264577 |
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| 출처 데이터셋 | uspto-grants-1993_11 |
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| ORD ID | ord-67075623cdb94f95b22545428d5c9080 |
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| 출처 메모 | uspto-grants-1993_11 |
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