関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrazole | HCID 1048 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Cyclohexanecarbonyl chloride | HCID 75938 | — |
| 反応物 | HCID 178418308 | HCID 178418308 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methoxy-5-methyl-6-(5-cyclohexylcarbonyloxy-1-ethylpyrazol-4-yl)carbonylthiochroman-1,1-dioxide | HCID 19693776 | 54% |
反応手順
As a starting material, 4-methoxy-5-methyl-6-(1-ethyl-5-hydroxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide corresponding to pyrazole derivative (I-H) was used. 0.4 Gram (1.1 mmol) thereof was dissolved in 4 ml of methylene chloride, and 0.22 g (2.2 mmol) of triethylamine as a base and 0.19 g (1.3 mmol) of cyclohexylcarbonyl chloride corresponding to compound B-A-Hal as a reaction reagent were added. The mixture was allowed to react at room temperature for 8 hours. A saturated sodium carbonate aqueous solution was added to the reaction mixture, and the resultant mixture was extracted with ethyl acetate. An organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the resultant oil was purified by flush column chromatography (Wako Gel C-300; hexane/ethyl acetate=1:1) to give 0.28 g (yield 54%) of 4-methoxy-5-methyl-6-(5-cyclohexylcarbonyloxy-1-ethylpyrazol-4-yl)carbonylthiochroman-1,1-dioxide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723408 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-3db0d270f6194dd0b5a468ba8e5ab869 |
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| 出典メモ | uspto-grants-1998_03 |
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