関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl 4-(2-oxopyridin-1(2H)-yl)benzoate | HCID 16656197 | — |
| 溶媒 | Oxolane--water (1/1) | HCID 21881883 | — |
| 生成物 | HCID 18453190 | HCID 18453190 | 85% |
反応手順
A mixture of ethyl 4-(2-oxopyridin-1(2H)-yl)benzoate (0.40 g, 1.64 mmol) and lithium hydroxide (0.28 g, 6.60 mmol) in tetrahydrofuran/water mixture was stirred at 70° C. for 1 h. The organic solvent was removed in vacuo. The water layer was washed with ethyl acetate (25 mL) and then acidified by addition of 15% hydrochloric acid solution. The solid obtained was collected by filtration, washed with water and dried in air to afford the title compound in 85% yield (0.30 g); 1H NMR (300 MHz, DMSO-d6) δ 13.14 (s, 1H), 8.02 (d, J=8.4 Hz, 2H), 7.65 (dd, J=1.9, 6.9 Hz, 1H), 7.51 (d, J=8.5 Hz, 2H), 7.48 (dd, J=1.9, 6.9 Hz, 1H), 6.47 (d, J=9.2 Hz, 1H), 6.31 (dt, J=1.0, 6.9 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541457B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-f97c14b776d44f2381eee4f0fc9630da |
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| 出典メモ | uspto-grants-2013_09 |
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