참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Methyl 6-iodo-5-(2-(thiophen-3-yl)ethoxy)nicotinate | HCID 57900415 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 3-Methylcarboxy-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepine | HCID 66869300 | 52.8% |
반응 단계
To a solution of 6-Iodo-5-(2-thiophen-3-yl-ethoxy)-nicotinic acid methyl ester (4.40 g, 11.3 mmol) in N,N-Dimethylformamide (176 mL, 2270 mmol) was added potassium carbonate (9.37 g, 67.8 mmol), triphenylphosphine (1.19 g, 4.52 mmol) and palladium acetate (508 mg, 2.26 mmol). The reaction mixture was stirred at 90° C. 8 h. The reaction mixture was diluted with MeOH then filtered through celite. The filtrate was concentrated. The crude product was purified by flash chromatography EtOAc/Hex (0-100%) (product eluted at 30%) to give 3-methylcarboxy-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepine (52.8%). MS: (ESI+) 262.0
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08399690B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_03 |
|---|
| ORD ID | ord-c598c3e4c4634fe8a9446b8b05f2025a |
|---|
| 출처 메모 | uspto-grants-2013_03 |
|---|
