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Pyrrolidine → 4-(Pyrrolidine-1-sulfonyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 4-(Chlorosulfonyl)benzoic acid | HCID 82385 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Pyrrolidine-1-sulfonyl)benzoic acid | HCID 763651 | 30.2% |
反応手順
To a solution of 4-chlorosulfonylbenzoic acid (2 g, 9.07 mmol) in dichloromethane (10 mL) was added a solution of pyrrolidine (1.29 g, 1.51 mL, 18.1 mmol) in dichloromethane (10 mL) and the reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was filtered and the white solid obtained was washed with water (50 ml) and diethyl ether (10 ml) and dried under vacuum to give 4-pyrrolidin-1-ylsulfonylbenzoic acid (700 mg, 30%). ESI-MS m/z calc. 255.0. Found 256.3 (M+1)+; Retention time: 1.18 minutes (3 min run); 1H NMR (400 MHz, DMSO) δ 13.49 (s, 1H), 8.15 (d, J=8.5 Hz, 2H), 7.92 (d, J=8.5 Hz, 2H), 3.17 (t, J=6.7 Hz, 4H), 1.65 (t, J=6.7 Hz, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828996B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-0485f254a93b4844907c5f29d2a44550 |
| 出典メモ | uspto-grants-2014_09 |