Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Hydroxide → 6-Oxo-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | Ammonium 6-oxo-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxylate | HCID 66971000 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-Oxo-3-(phenylamino)-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxamide | HCID 68457222 | 33.4% |
반응 단계
To a suspension of the compound of Example 14 (370 mg, 1.02 mmol) in anhydrous DMF (5 mL) was added 1,1′-carbonyldiimidazole (182 mg, 1.12 mmol) and the reaction stirred at r.t. under nitrogen for 20mins. Ammonium hydroxide (2 mL of 28% NH3 in water) was added and the reaction stirred for 72 h. Solvents were removed in vacuo and the crude residue purified by chromatography on silica (0-15% THF in DCM) to give the title compound as a white solid (123 mg). δH (DMSO-d6) 8.74 (1H, s), 7.67-7.34 (3H, m), 7.33-7.27 (2H, m), 7.22-7.00 (5H, m), 6.82-6.71 (3H, m), 6.21 (1H, d, J 9.7 Hz). LCMS (ES+) RT 3.04 minutes, 362 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07423047B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-f64a0912754e481195495f9dabe4999a |
| 출처 메모 | uspto-grants-2008_09 |