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Trifluoroacetic acid → 5-Bromochroman-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 2-Ethoxycarbonyl-5-bromo-3-chromanone | HCID 19043193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Bromochroman-3-one | HCID 19043186 | 53% |
反応手順
A suspension of 2-ethoxycarbonyl-5-bromo-3-chromanone (300 mg, 1 mMol) in methanol (5 mL) and 10% hydrochloric acid (3 mL) was heated at reflux for 2 hours. All of the solid had not dissolved; therefore, trifluoroacetic acid (1 mL) was added, and heating was continued for 18 hours. The reaction mixture was diluted with water and extracted well with diethyl ether. The ether phases were combined, dried over sodium sulfate, and concentrated in vacuo to give a yellow glass. Purification by flash chromatography (1:1 hexane:ether) gave the title compound as a light yellow glass (120 mg, 53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05340838 |
| 出典データセット | uspto-grants-1994_08 |
| ORD ID | ord-2ccc52b2841f499db61c2b94059b54ee |
| 出典メモ | uspto-grants-1994_08 |