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Diiodomethane → 2-Iodo-4-methyl-5-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diiodomethane | HCID 6346 | — |
| 反応物 | Isoamyl Nitrite | HCID 8053 | — |
| 反応物 | 2-Amino-4-methyl-5-nitropyridine | HCID 243165 | — |
| 生成物 | 2-Iodo-4-methyl-5-nitropyridine | HCID 23070167 | 28% |
反応手順
To a solution of 4-methyl-5-nitro-2-pyridinamine (12 g, 78.35 mmol) in diiodomethane (100 mL) was added isoamyl nitrite (22 mL, 160.4 mmol) at rt. After stirring for 30 min, the reaction was kept at 80° C. for 2 hr. The reaction was cooled and concentrated; but most of the diiodomethane remained. The crude mixture was loaded into column directly and eluted with 10% of EtOAc in hexane, and 2-iodo-4-methyl-5-nitropyridine (5.7 g, 28%) was obtained as a yellow solid after the removal of solvents under reduced pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198456B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-5829d3674d8c46e8b2bcfeb6c671fdd1 |
| 出典メモ | uspto-grants-2012_06 |