関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 3-[[4-(4-Acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrile | HCID 66699604 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 66699549 | HCID 66699549 | 93% |
反応手順
Stir a mixture of 3-[[4-(4-acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrile (13.4 g, 26.88 mmol), p-toluenesulfonic acid monohydrate (5.1 g, 26.88 mmol), methanol (100 mL), dichloromethane (50 mL), and ethyl acetate (50 mL) at room temperature for an hour. Concentrate the reaction mixture, dilute with ethyl acetate (150 mL) and wash with water (2×100 mL). Dry the organic phase over magnesium sulfate, filter, and concentrate. Dilute the residue with 5:1 hexanes:dichloromethane (50 mL), cool to 0° C. and filter. Collect a second and third crop to give the title compound (10.3 g, 93%), as a white solid. LCMS 416 M+1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07816523B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-faddbb6ac0d644f8850447eac37b3f1d |
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| 出典メモ | uspto-grants-2010_10 |
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