化工社化工社 化学情報印刷レポート · 研究参考用
N,N,N',N'-Tetramethylazodicarboxamide → Benzenepropanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N,N',N'-Tetramethylazodicarboxamide | HCID 4278 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | Benzenepropanol | HCID 31234 | — |
| 反応物 | N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-1,3-propylenediamine | HCID 21979958 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzenepropanol | HCID 31234 | — |
| 生成物 | N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-N'-(3-phenylpropyl)-1,3-propylenediamine | HCID 21979966 | — |
反応手順
A solution of Intermediate 1 (640 mg), 1,1′-azobis(N,N-dimethylformamide) (1200 mg, Aldrich or prepared according to Chemistry Letters, 539 (1994)) and 3-phenyl-1-propanol (710 μl, Tokyo Kasei Kogyo) in tetrahydrofuran (30 ml) was added with tri(n-butyl)phosphine (1.75 ml, Tokyo Kasei Kogyo) with stirring and ice cooling and stirred at room temperature under argon atmosphere for 13.5 hours. The precipitates in the reaction mixture were removed by filtration, and then the solvent was evaporated from the filtrate under reduced pressure. The residue was purified by flash column chromatography (hexane/ethyl acetate mixed solvent) to obtain the title compound (913 mg, mixture with a small amount of 3-phenyl-1-propanol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094789B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-99be45a0fb164c68b4577c67d8e9e37e |
| 出典メモ | uspto-grants-2006_08 |