化工社化工社 化学情報印刷レポート · 研究参考用
Thiophene, 2-nitro- → Ethyl 7-thienylamino-1H-pyrazolo[4,3-b]pyridine-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophene, 2-nitro- | HCID 11866 | — |
| 反応物 | 2-Aminothiophene | HCID 97373 | — |
| 反応物 | Ethyl 7-chloro-1H-pyrazolo[4,3-B]pyridine-6-carboxylate | HCID 20038759 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | Ethyl 7-thienylamino-1H-pyrazolo[4,3-b]pyridine-6-carboxylate | HCID 20156241 | 10.4% |
反応手順
Ethyl 7-chloro-1H-pyrazolo[4,3-b]pyridine-6-carboxylate (4.5 g 0.02 mole) and aminothiophene (2.0 g) [prepared from 2-nitrothiophene (supplied by Aldrich and shown by nmr to contain 15% of 3-nitrothiophene) by reduction using either H2 ; 10% Pd/C or stannous chloride] were stirred together under nitrogen for 24 hours. The ethanol was removed under reduced pressure. The resulting brown oil was purified by column chromatography on silica eluting with 5% methanol/ether to give the title compound as a beige solid (0.600 g), mp 188°-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04716160 |
| 出典データセット | uspto-grants-1987_12 |
| ORD ID | ord-40304c089c2d43628c76574169abe41e |
| 出典メモ | uspto-grants-1987_12 |