関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Amino-3-chlorobenzonitrile | HCID 519896 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloro-4-nitrobenzonitrile | HCID 14973028 | 90% |
反応手順
Sodium nitrite (6.78 g in water (40 mL) at 0° C.) was slowly added to a solution of 4-amino-3-chloro-benzonitrile (10.5 g) in water (30 mL) and concentrated hydrochloric acid (30 mL) also at 0° C. After 10 minutes the solution was poured onto a suspension of cuprous oxide (3.48 g) and sodium nitrite (31.69 g) in water (100 mL) at 0° C. The ensuing mixture was stirred at 0° C. for 1 hour then at 23° C. for 1 hour. The resulting mixture was extracted with dichloromethane and the organic layer washed with saturated sodium chloride. The separated organic layer was dried over sodium sulfate and then concentrated to give 3-chloro-4-nitro-benzonitrile (11.31 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06664395B2 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-69e7e0f0929e4c93a5729018f30478f0 |
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| 出典メモ | uspto-grants-2003_12 |
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