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Sodium Carbonate → N-(2,6-difluorophenyl)-3-[(8aS)-hexahydropyrrolo[1,2-a]pyrazin-2(1H)-ylcarbonyl]benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Benzoyl chloride, 3-(chlorosulfonyl)- | HCID 77671 | — |
| 反応物 | 2,6-Difluoroaniline | HCID 79647 | — |
| 反応物 | (6S)-1,4-Diazabicyclo(4.3.0)nonane | HCID 781249 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2,6-difluorophenyl)-3-[(8aS)-hexahydropyrrolo[1,2-a]pyrazin-2(1H)-ylcarbonyl]benzenesulfonamide | HCID 46853383 | — |
反応手順
To 3-(chlorosulfonyl)benzoyl chloride (0.474 g, 1.98 mmol) in anhydrous dichloromethane (10 mL) was added (S)-octahydropyrrolo[1,2-a]pyrazine (0.250 g, 1.98 mmol) in dichloromethane (4 mL) slowly over 10 minutes at room temperature. Then sodium carbonate (0.420 g, 3.96 mmol) was added. The mixture was stirred at room temperature for 5 hours. Then 2,6-difluoroaniline (2.56 g, 19.81 mmol) was added. The mixture was stirred at room temperature overnight and then concentrated. The residue was purified by chromatography on silica gel (dichloromethane, then methanol/dichloromethane=1:10) to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741899B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-7ba525e0068c4cafb6c8ebee64517b7d |
| 出典メモ | uspto-grants-2014_06 |