関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2,4,4'-Trihydroxydeoxybenzoin | HCID 640096 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Daidzein | HCID 5281708 | — |
反応手順
In a solution of 1-(2,4-dihydroxyphenyl)-2-(4-hydroxyphenyl)-ethanone (2 mmol) in DMF (6 mL), freshly distilled BF3.OEt2 (6.3 mL) was added under argon. The mixture was heated at 50° C., and a solution of methanesulphonyl chloride (1 mL) in dry DMF (1.5 mL) was added slowly. After reaction at 80° C. for 1 h, the mixture was cooled to rt and poured into a large volume of ice cold aq. sodium acetate (12 g/100 mL), then extracted with EtOAc, and the organic layer was dried and concentrated. The residue was purified by column chromatography on silica gel using a mixture of DCM and MeOH to give 7-hydroxy-3-(4-hydroxyphenyl)-chromen-4-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08093273B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-3389877a413e4f5c9170966b8d4af98a |
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| 出典メモ | uspto-grants-2012_01 |
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