関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 4'-Fluoro-2'-hydroxyacetophenone | HCID 2737326 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-fluoro-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran-4-one | HCID 15205373 | 70.7% |
反応手順
To 1-(4-fluoro-2-hydroxyphenyl)ethanone (5.75 g, 37.3 mmol) and propan-2-one (12 mL, 37.3 mmol) in benzene (50 mL) was added pyrrolidine (3.11 mL, 37.3 mmol) and the reaction heated at 80° C. for 3 hours. The reaction was diluted with ethyl acetate (50 mL), washed with 1N HCl (50 mL), brine (50 mL), dried over magnesium sulfate and concentrated. The residue was purified by silica gel chromatography, eluting with a gradient of 5% ethyl acetate/hexanes to 50% ethyl acetate, to provide the title compound (5.12 g, 70.7% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08569522B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-6d485f331b4747359a3d1a54b42eca6d |
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| 出典メモ | uspto-grants-2013_10 |
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