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Water → 4-Chloro-N-[1-(4-chlorobutanoyl)-1H-pyrazol-3-yl]butanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Phosphate, Dibasic | HCID 24450 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | HCID 178418806 | HCID 178418806 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Chloro-N-[1-(4-chlorobutanoyl)-1H-pyrazol-3-yl]butanamide | HCID 59794355 | 34% |
反応手順
To a solution of 3-aminopyrazole (300 mg, 3.61 mmol) in anh. CH2Cl2 (6 mL), at r.t., under N2, was added K2HPO4 (1.26 g, 2 eq) and the reaction mixture was stirred at r.t. for 15 min. 4-Chloro-butyryl chloride (406 μL, 3.6 mmol) was then added and the reaction mixture was stirred for 24 hr. It was then poured into water and the phases were separated. The aqueous layer was extracted with EtOAc (2×20 mL) and the combined organic extracts were dried over anh. Na2SO4. The solids were filtered and the solvent evaporated. The crude product was purified by flash chromatography (silica gel, cHex/EtOAc 7:3) to give the title compound as a white solid (354 mg, 34%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07427630B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-2154f7a9e0494f7ca847e5d03c3df2d0 |
| 出典メモ | uspto-grants-2008_09 |