참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-hydroxy-6,7,8,9-tetrahydro-5H-benzo[7]annulen-5-one | HCID 229507 | — |
| 반응물 | 1,1'-Biphenyl, 4-(bromomethyl)- | HCID 257716 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(4-phenylbenzyloxy)-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene | HCID 22989972 | 88% |
반응 단계
To 3-hydroxy-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene (1.76 g, 10.0 mmol) dissolved in DMF (20 ml) were added potassium carbonate (2.76 g, 20.0 mmol) and 4-phenylbenzyl bromide (2.72 g, 11.0 mmol), and the resulting mixture was stirred at room temperature for 24 hours. The reaction mixture was concentrated under reduced pressure, ethyl acetate (30 ml) and THF (30 ml) were added to the residue and the resulting mixture was washed with water (10 ml, 5 ml×3) and an aqueous saturated solution of sodium chloride (5 ml). The organic layer was dried with anhydrous magnesium sulfate and was then concentrated under reduced pressure, and the residue was mixed with diisopropyl ether, and an insoluble material was collected by filtration. The insoluble material was washed with diisopropyl ether and was then dried under reduced pressure to obtain 3-(4-phenylbenzyloxy)-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene (3.00 g, 8.76 mmol, 88%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06627651B1 |
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| 출처 데이터셋 | uspto-grants-2003_09 |
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| ORD ID | ord-1285b46a02434a35adefbb331b2aed8a |
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| 출처 메모 | uspto-grants-2003_09 |
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