関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1,3-Dichloro-5-methoxy-2,4,6-trinitrobenzene | HCID 14794057 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,3,5-Trichloro-2,4,6-trinitrobenzene | HCID 17518 | 95% |
反応手順
Thionyl chloride (0.20 ml, 0.027 mol) and dimethylformamide (0.15 ml, 0.022 mol) were added to a solution of 5 (0.624 g, 0.020 mol) in toluene (2 ml) at 50° C. The mixture was stirred and heated to 95° C. over a period of 15 min. and maintained at that temperature for another hour. The pale yellow solution was washed with water, dried over magnesium sulfate, treated with activated carbon, filtered, and evaporated to give a cream-colored solid (0.600 g, 95% yield). The melting point of the material so obtained was 194-195° C. (195-196° C. after recrystallization from acetic acid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04997987 |
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| 出典データセット | uspto-grants-1991_03 |
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| ORD ID | ord-6fd7ed6bceeb475aa404fdac8da39a05 |
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| 出典メモ | uspto-grants-1991_03 |
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