化工社化工社 化学情報印刷レポート · 研究参考用
N-(tert-Butoxycarbonyl)-1,5-diaminopentane → 4,5-Dihydro-4[5-(tert-butoxycarbonylamino)pentan-1-yl]-3H-1,4,8b-triazaacenaphthylen-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-(tert-Butoxycarbonyl)-1,5-diaminopentane | HCID 4352 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-[(Trimethylammonio)methyl]-5-ethoxycarbonylimidazo[1,2-a]pyridine iodide | HCID 21190128 | — |
| 生成物 | 4,5-Dihydro-4[5-(tert-butoxycarbonylamino)pentan-1-yl]-3H-1,4,8b-triazaacenaphthylen-5-one | HCID 21190173 | 54.8% |
反応手順
A solution of 7.78 g (20 mmol) of 3-[(trimethylammonio)methyl]-5-ethoxycarbonylimidazo [1,2-a]pyridine iodide, 6.07 g (30 mmol) of 5-tert-butoxycarbonylamino-1-pentylamine and 5.58 ml (40 mmol) of triethylamine was heated for 64 hours under reflux. The solvent was distilled off. To the residue was added methylene chloride, washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate/ethanol=10:1) to afford 3.93 g of the desired compound (54.9%, a pale yellow solid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05958942 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-fe3959d2b56d42c4b63412223c5abdc6 |
| 出典メモ | uspto-grants-1999_09 |