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, S and the solid product was collected by filtration 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 | US09006387B2 |
| 出典データセット | uspto-grants-2015_04 |
| ORD ID | ord-9f80fa95fee84f4f8a1b3dadd9dc502f |
| 出典メモ | uspto-grants-2015_04 |