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 | (Bromomethyl)cyclobutane | HCID 2734658 | — |
| 反応物 | HCID 178509603 | HCID 178509603 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Cyclobutylmethylthio-4-(3-trifluoromethylpyrazolyl)benzonitrile | HCID 178509605 | 21.6% |
反応手順
0.9 g (3.3 mmol) of 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile, 0.5 g (3.3 mmol) of cyclobutylmethyl bromide and 0.55 g (4.0 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at room temperature overnight. The resulting reaction mixture was poured into 50 ml of water and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, then washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 0.24 g of 2-cyclobutylmethylthio-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 21.2%) as a pale yellow powder (m.p. 102-103° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858639B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-109991864653475a9fb514957c60a928 |
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| 出典メモ | uspto-grants-2005_02 |
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