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Water → HCID 89962890、化合物
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 | 2,4-Difluoropyrimidine | HCID 137716 | — |
| 反応物 | HCID 89962731 | HCID 89962731 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 89962890 | HCID 89962890 | 51% |
反応手順
A solution of the 2,6-difluoro-4-{[(1S*,2R*)-2-(1-methyl-1H-pyrazol-5-yl)cyclopentyl]oxy}benzenesulfonamide (0.23 g, 0.65 mmol) prepared in Example 111c, 2,4-difluoropyrimidine (0.23 g, 1.96 mmol) and potassium carbonate (0.36 g, 2.61 mmol) in DMF (6.5 mL) was stirred at 120° C. for 3 hours. After allowing to cool, water (50 mL) was added to the reaction solution, followed by extraction with ethyl acetate (50 mL). The thus obtained organic layer was washed twice with water (50 mL) and dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography (ethyl acetate/methanol=6:1) to yield the title compound (150 mg, 51%) as a colorless amorphous solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889741B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-dfd2049633c94755aa00dccbf896d9a1 |
| 出典メモ | uspto-grants-2014_11 |