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 | HCID 9229 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Benzodioxole, 5-nitro- | HCID 75798 | 87.6% |
反応手順
1,3-Benzodioxole (10.0 g, 82 mmol) was added dropwise to a solution of con. HNO3 (65%-68%, 18 g) in H2O (39 g) at 6065° C. The mixture was then heated to 90° C. and stirred for 2 h at this temperature. The mixture was cooled to room temperature and poured into ice/water, filtered to give compound 5-nitrobenzo[d][1,3]dioxole (12.0 g, 87%) as a yellow solid. LCMS: 168 [M+1]+; 1H NMR (DMSO-d6) δ 6.27 (s, 2H), 7.12 (d, 1H, J=12 Hz), 7.76 (d, 1H, 3.2 Hz), 7.91 (dd, 1H, J1=12 Hz, J2=3.2 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040556B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-acc6ed9db35a4b989f84f11c6d1b2de1 |
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| 出典メモ | uspto-grants-2015_05 |
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