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Nitric Acid → 4-Methoxy-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 | 4-Methoxybenzo[d][1,3]dioxole | HCID 592478 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 4-Methoxy-6-nitro-1,3-benzodioxole | HCID 2825019 | 46% |
反応手順
4-Methoxy-benzo[1,3]dioxole (2.03 g, 13.34 mmole) was dissolved in acetic anhydride (20 mL) and cooled in an ice bath while stirring. Nitric acid (1.5 mL) was added dropwise with an addition funnel over 30 minutes. The ice bath was removed and the mixture was stirred overnight allowing the reaction to heat up to room temperature. The mixture was poured into ice water and the product crashed out and was filtered and washed with water. The precipitate was dried under vacuum in a dessicator yielding (1.21 g, 46% yield) of 4-methoxy-6-nitro-benzo[1,3]dioxole. NMR-DMSO-d6: 7.63 (s, 1H), 7.52 (s, 1H), 6.25 (s, 2H), 3.95 (s, 3H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902239B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-287c8eed20904c47bfb85e1d1d14d7e9 |
| 出典メモ | uspto-grants-2011_03 |