化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropyl Ether → N-(1,5-dimethylpyrazol-3-yl)-2,6 dimethyl benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | 2,6-Dimethylbenzoyl chloride | HCID 89096 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,5-dimethyl-1H-pyrazol-3-amine | HCID 7017747 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(1,5-dimethylpyrazol-3-yl)-2,6 dimethyl benzamide | HCID 11776550 | 38.2% |
反応手順
To a cooled (0°-5° C.) solution of 3-amino-1,5-dimethyl pyrazole (95%, 32.7 g, 0.28M) in anhydrous CH2Cl2 (200 ml) was added a CH2Cl2 (100 ml) solution of the 2,6 dimethyl benzoyl chloride (23.6 g, 0.14M). The reaction mixture was allowed to room temperature for 18 hours and then CH2Cl2 was concentrated to give an oily mixture which was diluted in AcOEt. This suspension was then treated with saturated NaHCO3. After usual work-up, the crude material was cristallized with diisopropyloxide to give 13 g of the desired amide (38% : yield based on the 2,6-dimethyl benzoyl chloride).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05464860 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-f98ffc91eb5e435fac5c17e51ecfdfc5 |
| 出典メモ | uspto-grants-1995_11 |