関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Potassium Permanganate | HCID 516875 | — |
| 反応物 | 1-(2-Chlorophenyl)-5-(furan-2-yl)-3-(trifluoromethyl)-1H-pyrazole | HCID 57458236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-chlorophenyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid | HCID 17960596 | — |
反応手順
An aqueous solution of 27.94 g of potassium permanganate in 100 ml of water was added dropwise to a mixture of 18.43 g of 1-(2-chlorophenyl)-5-(2-furyl)-3-trifluoromethyl-1H-pyrazole and 250 ml of acetone with being kept at 40° C. or lower. Then, the mixture was stirred at room temperature for 20 hours. The reaction mixture was filtered through Celite (registered trademark) to obtain a filtrate. The filtrate was adjusted to pH 10-12 by an addition of a 2N aqueous sodium hydroxide solution, and then extracted with ethyl acetate two times. The aqueous layer was adjusted to around pH 3 by an addition of 2 N hydrochloric acid, and then extracted with methyl tert-butyl ether three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and concentrated under reduced pressure to obtain 10.65 g of 1-(2-chlorophenyl)-3-trifluoromethyl-1H-pyrazole-5-carboxylic acid of the formula:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07867949B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-e7cb78fb2a8c4b68be55749e10866632 |
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| 出典メモ | uspto-grants-2011_01 |
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