関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Dimethylbenzenethiol | HCID 117548 | — |
| 反応物 | Dinitrobenzonitrile | HCID 520718 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[(3,5-Dimethylphenyl)thio]-6-nitrobenzonitrile | HCID 10613055 | 73,011.203% |
反応手順
A mixture of 2,6-dinitrobenzonitrile (1.4 g 7.2 mmol) and K2CO3 (1.1 g, 7.9 mmol) in 10 ml of DMF was chilled to 0° C. A solution of 3,5-dimethylthiophenol (1.1 g 0.0079 mmol) in 10 ml of DMF, was added dropwise over 30 min with stirring under nitrogen. After stirring an additional 30 min, the reaction mixture was poured into 150 ml of water and stirred for 1 hr. The solid was collected by vacuum filtration. Chromatography on silica gel (flash; Hex/EtOAc 1:1) provided 1.64 g (80%) of 2-[(3,5-dimethylphenyl)thio]-6-nitrobenzonitrile: mp 155°-156° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723452 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-942c876021324f25bb9887685a674993 |
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| 出典メモ | uspto-grants-1998_03 |
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