化工社化工社 化学情報印刷レポート · 研究参考用
Nitric Acid → 5-Methyl-6-nitro-1,3-benzodioxole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 1,3-Benzodioxole, 5-methyl- | HCID 81564 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Methyl-6-nitro-1,3-benzodioxole | HCID 4550461 | 64.4% |
反応手順
To a solution of 10 (19.0 g, 139.6 mmol) in acetic acid (180 mL) was added a solution of fuming HNO3 (10 mL) in acetic acid (70 mL) dropwise over 30 minutes. The mixture was stirred at ambient temperature for 10 minutes, then poured into a beaker containing ice to give a crystalline precipitate, which was collected by vacuum filtration and washed with water to afford the crude product. Further purification via recrystallization from CH2Cl2/hexane gave the pure product (16.3 g, 64.4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07122526B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-6b5c397707b34e689a13265ae5d3d2b4 |
| 出典メモ | uspto-grants-2006_10 |