関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Salicylate | HCID 8363 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,6-Di(propan-2-yl)phenyl carbonochloridate | HCID 271619 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Citric Acid | HCID 311 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Benzyl 2-[2,6-Bis(isopropyl)phenoxycarbonyloxy]-benzoate | HCID 21110017 | 57% |
反応手順
To a cooled (0° C.) solution of benzyl salicylate (0.77 g, 3.3 mmol) in dichloromethane (6 mL) was added triethylamine (0.52 mL, 3.7 mmol) and a catalytic amount of DMAP. To this mixture a suspension of compound (104) (0.9 g, 3.7 mmol, crude product from last step) in dichloromethane (4 mL) was further added. The reaction was allowed to warm to room temperature slowly and stirred for 14 h. The reaction mixture was then diluted with 10% aqueous citric acid solution (10 mL) and extracted with ethyl ether (2×40 mL). The organic phase was dried over MgSO4 and concentrated in vacuo. The residue was purified by radial chromatography on silica gel (eluting with ethyl acetate/hexane) to afford 0.8 g (57% yield over two steps) of the title compound (105).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07576127B2 |
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| 出典データセット | uspto-grants-2009_08 |
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| ORD ID | ord-274f4251ac5f470e866c915c104f7fc3 |
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| 出典メモ | uspto-grants-2009_08 |
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