関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1,3-Dihydroisobenzofuran | HCID 10327 | — |
| 反応物 | 1-Benzylpiperidine-4-carbaldehyde | HCID 89584 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Butyllithium | HCID 178418339 | — |
| 生成物 | (1-Benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanol | HCID 22248465 | 37.5% |
反応手順
After dissolving 591 mg of 1,3-dihydroisobenzofuran in 10 ml of tetrahydrofuran, 3.9 ml of n-butyllithium (1.5 M, n-hexane solution) was added thereto at −70° C. under a nitrogen atmosphere, the mixture was stirred for 1 hour, and then a solution of 1 g of 1-benzylpiperidine-4-carboxaldehyde in tetrahydrofuran (5 ml) was added dropwise and the mixture was stirred for 1 hour. Water was added to the reaction solution, extraction was performed with ethyl acetate, the extract was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. Purification was performed by silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain 597 mg of (1-benzylpiperidin-4-yl)-(1,3-dihydroisobenzofuran-1-yl)methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07915274B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-3cdf1cd5e0934747a1a5feee8f3dbe3e |
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| 出典メモ | uspto-grants-2011_03 |
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