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2-Nitrophenol → 1-Nitro-2-propoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Nitrophenol | HCID 6947 | — |
| 反応物 | 1-Bromopropane | HCID 7840 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Nitro-2-propoxybenzene | HCID 587497 | 87% |
反応手順
o-Nitrophenol (111.2 g., 0.8 mole), 1-bromopropane (98.4 g., 0.8 mole), anhydrous potassium carbonate (121.4 g., 0.88 mole) and any acetone (800 cc) are refluxed for 70 hrs., filtered the reaction mass, the residue was washed with acetone, and the filtrate rotoevaporated. To the residue of the evaporation was added 200 cc of dichloromethane and rotoevaporated again; the residue was washed with 100 cc of water and separated into two layers. The dichloromethane layer was washed with 100 cc of 10% Na2CO3, separated again, washed again with 100 cc of water, and the dichloromethane layer was fractionated under vacuum. The main fraction distilled at 103°-106° C. at 0.2-0.3 mm Hg., giving 130 g. of product (87% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04345937 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-c50366e1aaf143d88d8f60c298b18d14 |
| 出典メモ | uspto-grants-1982_08 |