関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 5-Chloro-2,3-dihydro-1-benzofuran | HCID 592964 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Chloro-7-nitro-2,3-dihydro-1-benzofuran | HCID 18997244 | 40.5% |
反応手順
To a stirred and cooled mixture of 32 ml of sulfuric acid and 14 ml of water there were added 17 g of 2,3-dihydro-5-chlorobenzofuran, while keeping the temperature at 25° C. After cooling to 0° C. there were added dropwise 14 ml of nitric acid. Stirring and cooling at 0° C. was continued for 44 hours. The reaction mixture was diluted with water (temp. <10° C.) and stirred for 15 min. The precipitate was filtered off, washed with water and recrystallized from a mixture of ethyl acetate and hexane (30:70), yielding 8.9 g (40.5%) of 5-chloro-2,3-dihydro-7-nitrobenzofuran (interm. 3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05480912 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-417de0039c7b4e3f9ac70af45c0a5b10 |
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| 出典メモ | uspto-grants-1996_01 |
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