化工社化工社 化学情報印刷レポート · 研究参考用
Diethyl Ether → 4'-Dimethylaminoacetanilide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | N,N-dimethyl-p-phenylenediamine | HCID 7472 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4'-Dimethylaminoacetanilide | HCID 81968 | 86% |
反応手順
To a solution of acetic anhydride (11.5 mL, 12.45 g, 0.122 mol) in anhydrous CH2Cl2 (100 mL) was added N,N-dimethyl-1,4-phenylenediamine (11.37 g; 83.5 mmol) portion-wise over 30 min at 0° C. The mixture was allowed to gradually warm to room temperature and stirred for 24 hours. The solvent was removed under high vacuum to obtain a black residue which was stirred with Et2O (20 mL) at room temperature. The suspension was filtered and the solid washed with Et2O (3×20 mL). The solid residue was dried under high vacuum to obtain the intermediate N-acetyl-N′,N′-dimethyl-1,4-phenylenediamine as a black solid (12.8 g, 86%) which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09340498B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-8fe6959594ae47a78180183b92f8aedb |
| 出典メモ | uspto-grants-2016_05 |