참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 3-{3-[(Dibenzofuran-2-carbonyl)-amino]-phenyl}-acrylic acid ethyl ester | HCID 68413672 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 3-{3-[(Dibenzofuran-2-carbonyl)-amino]phenyl}-acrylic acid | HCID 68412257 | — |
반응 단계
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)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08080567B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-7ad11f1219ac4ba68972f8d9b5a47837 |
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| 출처 메모 | uspto-grants-2011_12 |
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