5-hydroxy-8-methoxy-3,4-dihydro-2H-naphthalen-1-one → HCID 21255658、化合物
反応式
[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]=1参加物
3
反応条件
- 温度
- 0 °C
実験手順
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).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-6176022d31614c67844137558d757a14
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06194454B1
反応ノート
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