化工社化工社 化学情報印刷レポート · 研究参考用
m-Fluorotoluene → 5-Fluoro-2-nitrotoluene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Fluorotoluene | HCID 9606 | — |
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 5-Fluoro-2-nitrotoluene | HCID 94956 | — |
反応手順
3-Fluorotoluene (1 mole) in concentrated sulfuric acid (200 ml.) is stirred at 0° C. while a cold solution of potassium nitrate (1.5 mole) in concentrated sulfuric acid (750 ml.) is added slowly during 3 hours, the temperature being kept below 5° C. with an ice-ethanol bath After the addition is complete, the ice-bath is removed and stirring is continued for 3 hours at room temperature. Water (400 ml.) is added, and the organic layer is separated, dried (MgSO4) and filtered. The oil is separated by vapor-phase chromatograph on a 200×1 cm. silicone oil column (DC 200 20%) on Chromosorb R (60/80) at 191° C. and a helium flow rate of 86 ml./min. The desired pure nitro-isomer is collected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06020379 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-e0580b885415450aac93fae5585ef695 |
| 出典メモ | uspto-grants-2000_02 |