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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 | Chloroform | HCID 6212 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Methyl-6-nitro-1,3-benzodioxole | HCID 4550461 | 90% |
反応手順
5-Methyl-1,3-benzodioxole (8.00 g, 58.8 mmol) was dissolved in chloroform (160 ml), and the mixture was stirred under ice-cooling. To this solution was gradually added 60% nitric acid (20 ml), and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with dichloromethane, washed with water and saturated aqueous sodium hydrogen carbonate, and dried over potassium carbonate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give the title compound (9.58 g, yield 90%) as a pale-yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08513235B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-d622537d0d57496f8d10b97bbaadf49d |
| 出典メモ | uspto-grants-2013_08 |