化工社化工社 化学情報印刷レポート · 研究参考用
tert-Butanol → 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | 4'-Chloro-3'-nitroacetophenone | HCID 79596 | — |
| 反応物 | 2-Bromo-1-(4-chloro-3-nitrophenyl)ethan-1-one | HCID 2778330 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-dione | HCID 86649099 | — |
反応手順
Zinc chloride (27.4 g, 201 mmol), diethylamine (15.6 mL, 151 mmol) and t-butanol (14.4 mL, 151 mmol) were combined in benzene (151 mL) at room temperature under a nitrogen atmosphere and stirred for 2 h. 1-(4-chloro-3-nitrophenyl)ethanone (30.1 g, 151 mmol) and 2-bromo-1-(4-chloro-3-nitrophenyl)ethanone (28 g, 101 mmol) were added. The mixture was stirred vigorously for 20 h, and the solid product was collected by filteration and rinsed with benzene, water, methanol, and dichloromethane. The solid was dried in a vacuum oven.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08691938B2 |
| 出典データセット | uspto-grants-2014_04 |
| ORD ID | ord-108a162284974588bcea8ba907eebf9d |
| 出典メモ | uspto-grants-2014_04 |