関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N,N-Dimethylpiperidin-4-amine | HCID 417391 | — |
| 反応物 | 2-Chloro-5-pyridinesulfonyl chloride | HCID 2792792 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[(6-chloro-3-pyridinyl)sulfonyl]-N,N-dimethyl-4-Piperidinamine | HCID 43430609 | 94.5% |
反応手順
To a stirred ice-cooled solution of 4-(dimethylamino)piperidine (1.2 mL, 9.4 mmol), triethylamine (2.6 mL, 19 mmol), and 4-dimethylaminopyridine (0.012 g, 0.094 mmol) in DCM (18 mL) was added 6-chloropyridine-3-sulfonyl chloride (2.0 g, 9.4 mmol) in one portion. The resulting mixture was stirred at 0° C. for 1.5 h. Upon workup, the mixture was directly subjected to combi-flash column chromatography (methanol/DCM) to give compound 363 (2.7 g, 94% yield) as a white solid. LCMS-ESI (POS), M/Z, M+1: Found 304.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841312B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-f167625d6b5544b1b197359d6bc6ec00 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
