関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorodifluoromethane | HCID 6372 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 178498595 | HCID 178498595 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate | HCID 54319416 | — |
反応手順
67.6 g (0.43 mol) 5-Hydroxy-3-methoxycarbonyl-1-methylpyrazole and 299.2 g (2.17 mol) potassium carbonate was dissolved in 1500 ml dimethylformamide and heated to 70° C. At this temperature chlorodifluoromethane was introduced over 2 hours and the mixture stirred at 80° C. for 1.5 hours. The reaction mixture was added to water and extracted 6 times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The reaction solution was concentrated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05869686 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-00d102e2297d4b64bd63ab720ce4305c |
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| 出典メモ | uspto-grants-1999_02 |
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