5-hydroxy-8-methoxy-3,4-dihydro-2H-naphthalen-1-one → HCID 21255658, 화합물
반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=O>FC(F)(F)C(O)=O>[CH3:13][O:12][C:9]1[C:8]2[CH2:7][CH2:6][CH2:5][CH2:4][C:3]=2[C:2]([OH:1])=[CH:11][CH:10]=1참가 물질
3
반응 조건
- 온도
- 0 °C
실험 절차
To a cooled (0° C.), stirred solution of 5-hydroxy-8-methoxy-3,4-dihydro-2H-naphthalen-1-one (1.7 g) in trifluoroacetic acid (20 mL) triethylsilane (4.2 mL) was added and the reaction warmed to RT and then stirred for 1.5 h). The reaction mixture was concentrated in vacuo, partitioned between ethyl acetate/water, the organic layer was washed with water, brine, and then dried over sodium sulfate and concentrated in vacuo. The resulting oil is flash chromatographed (10% ethyl acetate/hexanes) to afford the title compound as a colorless solid (1.6 g).
후처리
- additionwas added
- temperaturethe reaction warmed to RT
- concentrationThe reaction mixture was concentrated in vacuo
- custompartitioned between ethyl acetate/water
- washthe organic layer was washed with water, brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customchromatographed (10% ethyl acetate/hexanes)
출처 및 근거
- ORD 기록
- ord-6176022d31614c67844137558d757a14
- 출처 데이터셋
- uspto-grants-2001_02
- 특허 번호
- US06194454B1
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