化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → beta-cyano-N-(2,4,6-trimethoxyphenyl)benzene propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2,4,6-Trimethoxyaniline | HCID 84271 | — |
| 反応物 | 3-Cyano-3-phenylpropanoic acid | HCID 11194625 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | beta-cyano-N-(2,4,6-trimethoxyphenyl)benzene propanamide | HCID 86748282 | — |
反応手順
To a dichloromethane (150 mL) solution of 3-cyano-3-phenylpropionic acid (5 g, 0.0286 mol) at 0° C. under a nitrogen atmosphere was added triethylamine (4 mL, 0.0286 mol) and 2,4,6-trimethoxyaniline.HCl (6.3 g, 0.0286 mol). To this solution was added DCC (6.2 g, 0.29 mol). The resulting mixture was allowed to warm to room temperature over 3 hours. This was then filtered and the filtrate partitioned between 1N HCl and dichloromethane. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The resulting solid (5.1 g) was recrystallized from dichloromethane/hexanes, mpt 157°-160° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05646170 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-d32b4e3cf5d2438cb998495b505814f9 |
| 出典メモ | uspto-grants-1997_07 |