化工社化工社 化学情報印刷レポート · 研究参考用
Homoveratrylamine → SB-237376
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Homoveratrylamine | HCID 8421 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-(3-chloropropyl)-4-nitrobenzamide | HCID 3421653 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | SB-237376 | HCID 9845213 | 23.6% |
反応手順
A solution of 10.62 g (44 mmol) N-(3-chloropropyl)-4-nitrobenzamide (D3), 8.1 g (45 mmol) homoveratrylamine and 6.26 ml triethylamine in 200 ml methylene chloride was refluxed for 48 h. The solvent was then concentrated in vacuo and the residue dissolved in water. The aqueous phase was first washed with methylene chloride, then made basic with aqueous NaOH and finally extracted twice with methylene chloride. This second organic phase was dried over MgSO4 and concentrated in vacuo affording 12 g of a crude residue. This residue was purified by chromatography on silicagel using CH2Cl2 /MeOH/NH4OH: 85/10/5 to afford 4.4 g of the title compound as an yellow oil (free base).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05977179 |
| 出典データセット | uspto-grants-1999_11 |
| ORD ID | ord-23ba9b4686454633b0a023f2fe66b624 |
| 出典メモ | uspto-grants-1999_11 |