참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Ethyl 6-bromonaphthalene-2-carboxylate | HCID 1249959 | — |
| 반응물 | (5,6,7,8-Tetrahydro-5,5-dimethylnaphth-2-yl)boronic acid | HCID 22571498 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Sodium Carbonate | HCID 10340 | — |
| 생성물 | Ethyl-6-[5,6,7,8-tetrahydro-5,5-dimethyl-naphth-7-yl]naphth-2-oate | HCID 22571563 | — |
반응 단계
To a degassed solution of 0.39 g (1.4 mmol) of ethyl 6-bromo-naphthalene-2-carboxylate and 3.0 mL of toluene, was added sequentially 49 mg (0.04 mmol) of tetrakis-triphenylphosphine palladium(0), 2.0 mL (2.0 mmol) of 1M sodium carbonate and then a solution of 0.32 g (1.6 mmol) of (5,6,7,8-tetrahydro-5,5-dimethylnaphth-2-yl)boronic acid (Compound B13) in 3.0 mL of MeOH. The reaction was heated at 80° C. for 6 h, diluted with 2N Na2CO3, and extracted with CH2Cl2 (2×), the organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo to give an oil. Flash chromatography (silica, 5% ethyl acetate in hexane) of the crude material gave the title compound as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06187933B1 |
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| 출처 데이터셋 | uspto-grants-2001_02 |
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| ORD ID | ord-a2eaf539bd85402d91e916b30fb3ac63 |
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| 출처 메모 | uspto-grants-2001_02 |
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