関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromopropane | HCID 6358 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 4-Hydroxy-3-(trifluoromethyl)benzoic acid | HCID 2775112 | — |
| 生成物 | Isopropyl 4-isopropoxy-3-(trifluoromethyl)benzoate | HCID 59201795 | — |
反応手順
To a mixture of 4-hydroxy-3-(trifluoromethyl)benzoic acid (14.55 mmol) and cesium carbonate (43.7 mmol) in DMA (60 mL) was added 2-bromopropane (36.4 mmol). The reaction was stirred at 80° C. for 16 h. The mixture was filtered through celite and concentrated under vacuum. The residue was dissolved in EtOAc and washed with water, then brine, then dried over MgSO4, and filtered. The solvent was removed under vacuum to give the title compound as a light yellow oil (13.1 mmol). 1H NMR (400 MHz, CDCl3) δ ppm 1.36 (d, J=6.32 Hz, 6H), 1.39 (d, J=6.06 Hz, 6H), 4.72 (septet, J=6.06 Hz, 1H), 5.24 (septet, J=6.25 Hz, 1H), 7.00 (d, J=8.84 Hz, 1H), 7.26 (s, OH), 8.15 (dd, J=8.72, 2.15 Hz, 1H), 8.23 (d, J=2.15 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09108969B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-9981af631bc54817bb8e387e9116ac2e |
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| 出典メモ | uspto-grants-2015_08 |
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