化工社化工社 化学情報印刷レポート · 研究参考用
Diethylamine → 4-benzoyl-N,N-diethylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-Benzoylbenzoic acid | HCID 69147 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 4-benzoyl-N,N-diethylbenzamide | HCID 755990 | 95.5% |
反応手順
A solution of 25 g (110 mmol) 4-benzoylbenzoic acid [611-95-0] and 20 mL SOCl2 was allowed to reflux for 2 h then allowed to cool. The excess SOCl2 was evaporated off and the resulting clear oil was dissolved in 10 mL CH2Cl2 then slowly added to 12 mL (116 mmol) diethylamine in a mixture of 10 mL 3N NaOH and 50 mL CH2Cl2. The mixture was allowed to stir for 30 min then partitioned between H2O and CH2Cl2. The organic layer was washed with brine, dried over K2CO3, filtered and concentrated. The product precipitated from EtOAc/hexane to give 29.6 g (105 mmol) white crystals. MS m/z (MH+) 282.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06552036B2 |
| 出典データセット | uspto-grants-2003_04 |
| ORD ID | ord-b6906a990c194f889bb665cdfe1b54fa |
| 出典メモ | uspto-grants-2003_04 |