참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Fluoro-5-(trifluoromethyl)aniline | HCID 136349 | — |
| 반응물 | Trimethylaluminum | HCID 16682925 | — |
| 반응물 | HCID 178496995 | HCID 178496995 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 178522155 | HCID 178522155 | 17.5% |
반응 단계
To a solution of methyl 7-((2-chloro-6-fluorophenyl)amino)-2-cyclopropyl-8H-imidazo[4′,5′:5,6]-benzo[1,2-d]oxazole-4-carboxylate (Intermediate-59, 0.050 g, 0.125 mmol) in dry toluene (5.0 mL) was added 2-fluoro-5-trifluoromethylaniline (0.022 g, 0.125 mmol) and trimethyl aluminium (2M solution in toluene) (0.009 g, 0.125 mmol). The reaction mass was refluxed for 1 h. The reaction mass was quenched with water and extracted with 10% DCM: MeOH. The organic layer was dried over anhydrous sodium sulphate and concentrated. The obtained crude was purified by column chromatography to afford 0.012 g of the desired product. 1HNMR (DMSO-d6): δ 1.23 (m, 4H), 2.33 (m, 1H), 7.40-7.47 (m, 3H), 7.62 (m, 2H), 7.75 (s, 1H), 8.68 (s, 1H), 9.42 (s, 1H), 9.89 (s, 1H), 11.69 (s, 1H); MS [M+H]+: 547.81.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08519149B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-68ced7b6868849c2af2ff7d968dd1a93 |
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| 출처 메모 | uspto-grants-2013_08 |
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