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HRID 1967151作成日：2026年10月26日
Potassium Carbonate → 5-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-{[4-(methylsulfonyl)phenyl]amino}thiophene-3-carboxamide
https://huagongshe.com/reaction/1967151
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-(methylsulphonyl)benzene | HCID 77014 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | 2-Amino-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]thiophene-3-carboxamide | HCID 59525619 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-{[4-(methylsulfonyl)phenyl]amino}thiophene-3-carboxamide | HCID 44610063 | — |
反応手順
2-amino-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]thiophene-3-carboxamide (0.1 g, 0.320 mmol), 4-bromophenyl methyl sulfone (0.075 g, 0.320 mmol), Pd2 dba3 (0.029 g, 0.032 mmol), K2CO3 (0.049 g, 0.352 mmol) and X-Phos (0.076 g, 0.160 mmol) were added to a 5 mL microwave vial. Degassed EtOH (1 mL) was added and the vial evacuated and back-filled with N2 (×3). The resulting mixture was stirred at 100° C. overnight. Room temperature was attained, MeOH was added and the solvent removed in vacuo while loading onto silica. Purification of the residue by MPLC (0-10% MeOH—CHCl3) gave 5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-{[4-(methylsulfonyl)phenyl]amino}thiophene-3-carboxamide as a beige solid after triturating in DCM.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08420695B2 |
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| 出典データセット | uspto-grants-2013_04 |
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| ORD ID | ord-3990bd39f71a43ddafd560707804bd84 |
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| 出典メモ | uspto-grants-2013_04 |
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