HCID 67126235, 화합물 → 6-Chloro-7-fluoro-3-methylnaphthalen-1-ol
반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([CH3:17])=[CH:11][C:12]([O:14]CC)=O)[CH:5]=[CH:6][C:7]=1[F:8]>S(=O)(=O)(O)O.O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[F:8])[C:12]([OH:14])=[CH:11][C:10]([CH3:17])=[CH:9]2참가 물질
4
실험 절차
A solution of ethyl 4-(3-chloro-4-fluorophenyl)-3-methylbut-2-enoate (9.7 g, 37.8 mmol) in concentrated sulfuric acid (40 mL) was stirred at 50° C. overnight. The reaction mixture was poured onto ice and diluted with water and extracted with ethyl acetate. The organic layer was concentrated and purified by flash column chromatography (silica gel, ethyl acetate/hexanes) to give a pale yellow solid (1.57 g). 1H-NMR: 400 MHz, (CDCl3) δ: 7.83 (d, J=10.4 Hz, 1H), 7.75 (d, J=7.2 Hz, 1H), 7.11 (s, 1H), 6.67 (s, 1H), 2.42 (s, 3H).
후처리
- additionThe reaction mixture was poured onto ice
- extractionextracted with ethyl acetate
- concentrationThe organic layer was concentrated
- custompurified by flash column chromatography (silica gel, ethyl acetate/hexanes)
출처 및 근거
- ORD 기록
- ord-db69d8db1fe649929295841ccf6acb45
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09102614B2
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