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5-Bromothiophene-2-sulfonyl chloride → 5-Bromo-N-{5-(cis-3,5-dimethyl-1-piperazinyl)-2-[(phenylmethyl)oxy]phenyl]-2-thiophenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Bromothiophene-2-sulfonyl chloride | HCID 2733924 | — |
| 反応物 | 5-(cis-3,5-Dimethyl-1-piperazinyl)-2-[(phenylmethyl)oxy]aniline | HCID 59007092 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-N-{5-(cis-3,5-dimethyl-1-piperazinyl)-2-[(phenylmethyl)oxy]phenyl]-2-thiophenesulfonamide | HCID 59007096 | — |
反応手順
A solution of 5-(cis-3,5-dimethyl-1-piperazinyl)-2-[(phenylmethyl)oxy]aniline (D39) (300 mg, 0.96 mmol) in dichloromethane (5 ml) and pyridine (5 ml) was added 5-bromo-2-thiophenesulfonyl chloride (505 mg, 1.93 mmol) and the mixture stirred at room temperature for 4 hours. The mixture was then reduced in vacuo and the residue purified by SCX (eluting with methanol then ammonia 2M in methanol). The appropriate fractions were combined and reduced and the residue purified by trituaration with methanol to afford the title compound (D42). MS (ES+) m/e 536/538 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381728B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-4ecedd6316164cc78f6a55d979f81622 |
| 出典メモ | uspto-grants-2008_06 |