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-carboxylic acid | HCID 7196 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 6-Nitro-1,3-benzodioxole-5-carboxylic acid | HCID 246435 | 92% |
反応手順
To 5-carboxy-1,3-benzodioxole (50 g, 300 mmol) in trifluoroacetic acid (400 mL) at 0° C. was added HNO3 (38 mL, 900 mmol) dropwise. The reaction mixture was stirred at 0° C. for 1 hour, then warmed to ambient temperature and stirred for 3 hours. The mixture was poured into ice water and the resulting precipitate was collected by filtration. The solid was air dried overnight to afford 58 g (92% yield) of 5-carboxy-6-nitro-1,3-benzodioxole as a yellow solid; NMR (DMSO-d6) 7.6 (s, 1), 7.3 (s, 1), 6.3 (s, 2) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06380221B1 |
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| 出典データセット | uspto-grants-2002_04 |
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| ORD ID | ord-eada0339c38a4e47af9114b0d8da3934 |
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| 出典メモ | uspto-grants-2002_04 |
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