関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-Chloro-5-nitrobenzoic acid | HCID 17287 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 生成物 | 2-Chloro-5-nitrobenzamide | HCID 286562 | — |
反応手順
A mixture of 2-chloro-5-nitrobenzoic acid (15.0 g, 74.0 mmol) and 200 mL of dichloromethane was reacted with oxalyl chloride (16.2 mL, 186.0 mmol) and a catalytic amount of dimethylformamide. The mixture was stirred at 25° C. for 3 hours. The solvent was removed in vacuo, and the residue was redissolved in 200 mL of dichloromethane. The solution was cooled to 0° C., and ammonia was bubbled through the cold solution for 5 minutes, whereupon the product precipitated to form solution. The product was collected by filtration to yield 6.8 g, mp 174°-175° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05620997 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-c5cf0b48a4a34299955db292eb81bf2e |
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| 出典メモ | uspto-grants-1997_04 |
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