関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 3-{3-[(Dibenzofuran-2-carbonyl)-amino]-phenyl}-acrylic acid ethyl ester | HCID 68413672 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 3-{3-[(Dibenzofuran-2-carbonyl)-amino]phenyl}-acrylic acid | HCID 68412257 | — |
反応手順
The ester (19) (46 mg, 0.12 mmol) was hydrolysed using Method C, except that MeOH (1 mL) and THF (1 mL) were used, and the reaction mixture was heated to 40° C. for 1 hour. After the reaction, TBME was added and the mixture acidified using 6N HCl. The aqueous was extracted with more TBME (×3), EtOAc (×3), dried (MgSO4) and the solvent concentrated in vacuo. The crude solid was triturated with DCM, filtered, washed with heptane and dried to give the title compound. Yield: 34 mg, 81%; LC-MS tr 2.08 min; HPLC Purity: 100%; MS (ES+) m/z 358 (M+H); 1H NMR (400 MHz; DMSO): δ 6.60 (d, 1H), 7.55-7.75 (m, 5H), 7.9 (d, 1H), 7.95-8.05 (m, 2H), 8.25 (s, 1H), 8.30 (d, 1H), 8.40 (d, 1H), 8.95 (s, 1H), 10.65 (s, 1H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08080567B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-7ad11f1219ac4ba68972f8d9b5a47837 |
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| 出典メモ | uspto-grants-2011_12 |
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