関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Methyl 6-iodo-5-(2-(thiophen-3-yl)ethoxy)nicotinate | HCID 57900415 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Methylcarboxy-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepine | HCID 66869300 | 52.8% |
反応手順
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
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07928248B2 |
|---|
| 出典データセット | uspto-grants-2011_04 |
|---|
| ORD ID | ord-eee2841813c945a1b7021c08353f4f4d |
|---|
| 出典メモ | uspto-grants-2011_04 |
|---|
