関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 2-Benzhydryl-2H-pyran-4(3H)-one | HCID 66630848 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | trans-2-Benzhydryl-tetrahydropyran-4-ol | HCID 66631792 | 68% |
反応手順
NaCNBH3 (0.75 g, 12 mmol) was added portionwise to a mixture of 2-diphenylmethyl-2,3-dihydro-4H-pyran-4-one 2 (1.05 g, 4 mmol) and boron trifluoride etherate (1.99 g, 14 mmol) in dry THF (50 ml) cooled to −78° C. The reaction mixture was allowed to reach room temperature and the reaction was quenched with saturated aqueous NaHCO3 (30 ml). The organic phase was separated, and the aqueous phase was extracted with ethyl ether (3×20 ml). The organic phases were combined and dried over anhydrous Na2SO4. Removal of the solvent under reduced pressure, and purification by flash chromatography (hexane/ethyl acetate 7:3) first afforded trans-2-benzhydryl-tetrahydropyran-4-ol 3a (0.73 g, 68% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08017791B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-7bec885c091142e4ad19e0d0b3334900 |
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| 出典メモ | uspto-grants-2011_09 |
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