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Benzoic acid, 3-(chlorosulfonyl)- → 3-{[[(3-Bromophenyl)methyl](methyl)amino]sulfonyl}benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic acid, 3-(chlorosulfonyl)- | HCID 77641 | — |
| 反応物 | Benzenemethanamine, 3-bromo-N-methyl- | HCID 457588 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-{[[(3-Bromophenyl)methyl](methyl)amino]sulfonyl}benzoic acid | HCID 57813251 | 78.3% |
反応手順
1-(3-Bromophenyl)-N-methylmethanamine (0.100 g, 0.5 mmol) in DCM (5 mL) was added TEA (0.139 mL, 1.000 mmol) and 3-(chlorosulfonyl)benzoic acid (0.110 g, 0.500 mmol). The resulting mixture was stirred at room temperature for 0.5 h. The reaction was quenched with HCl (1 N), concentrated and redissolved in EtOAc (10 mL) which was washed with H2O (2×3 mL), brine (3 mL), then dried with Na2SO4. It was then filtered and concentrated to afford the title compound (0.1505 g, 78%). LC-MS m/z 384 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08067408B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-caa4573a80e24f40a34fe6341b29b0f6 |
| 出典メモ | uspto-grants-2011_11 |