참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Ethyl 3-(phenylamino)-6-oxo-7-phenyl-6,7-dihydrothieno[2,3-b]pyridine-2-carboxylate | HCID 9865198 | — |
| 용매 | 1-Ethoxyethanol | HCID 10129898 | — |
| 생성물 | HCID 68454135 | HCID 68454135 | 46% |
반응 단계
To a stirred solution of Example 1 (200 mg, 0.5 mmol) in ethoxyethanol (5 mL) was added hydrazine hydrate (1.5 mmol). The reaction mixture was heated to 120° C. for 6 h. Upon cooling the reaction mixture was poured into sat NaHCO3 aq and extracted with DCM (×2). The combined organic fractions were dried (MgSO4) and concentrated in vacuo. Purification by flash column chromatography (silica, 5% EtOH in DCM) gave the title compound (86 mg, 46%). δH (CDCl3) 8.76 (1H, br s), 8.60 (1H, br s), 7.55-7.7 (3H, m), 7.4-7.5 (2H, m), 7.25-7.35 (3H, m), 6.9-7.0 (2H, m), 6.35 (1H, d, J 10 Hz), 4.3 (2H, br s). LCMS (ES+) RT 2.84 minutes, 377 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07763729B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_07 |
|---|
| ORD ID | ord-297f06aaec354215ad402a5e7adb2fab |
|---|
| 출처 메모 | uspto-grants-2010_07 |
|---|
