関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | (1-Benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanol | HCID 22248465 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (1-Benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanone | HCID 22248144 | 87.1% |
反応手順
After adding 0.511 ml of dimethylsulfoxide dropwise to a dichloromethane solution (15 ml) containing 0.315 ml of oxalyl chloride at −70° C., the mixture was stirred for 10 minutes, a solution of 597 mg of (1-benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanol in dichloromethane (5 ml) was added dropwise, and stirring was continued for 1 hour. Next, 2.5 ml of triethylamine was added dropwise to the reaction solution, the cooling bath was removed, and the mixture was stirred at room temperature. Water was added to the reaction solution, and extraction was is performed with ethyl acetate. After drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure to obtain the title compound (517 mg, 33% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06995144B2 |
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| 出典データセット | uspto-grants-2006_02 |
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| ORD ID | ord-29889e375efc40a0b71c63ca6bfbdef9 |
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| 出典メモ | uspto-grants-2006_02 |
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