化工社化工社 化学情報印刷レポート · 研究参考用
Isoamyl nitrate → Methyl 4-iodo-1H-indazole-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isoamyl nitrate | HCID 10985 | — |
| 反応物 | HCID 67512060 | HCID 67512060 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 4-iodo-1H-indazole-6-carboxylate | HCID 24728119 | 91% |
反応手順
To a solution of 3-amino-5-iodo-4-methyl-benzoic acid methyl ester (1.22 g, 4.21 mmol) in acetic acid (20 mL) was added isoamyl nitrate (0.675 mL, 4.63 mmol). The mixture was stirred at room temperature for 30 minutes and then concentrated under reduced pressure. The residue was partitioned between dichloromethane and saturated aqueous sodium bicarbonate. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography to give 1.15 g (91%) of 4-iodo-1H-indazole-6-carboxylic acid methyl ester, MS (M+H)=303.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440956B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-70809c7613524ef497c67b64df382b7e |
| 出典メモ | uspto-grants-2016_09 |