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Hydrochloride methanol → 4-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloride methanol | HCID 21893726 | — |
| 反応物 | tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate | HCID 59166177 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride | HCID 67133869 | 71% |
反応手順
To a solution of tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate (8.5 g, 23.4 mmol) in MeOH (10 mL) was added HCl/MeOH (2M, 50 mL) at room temperature. The suspension was stirred at room temperature overnight. The solid product was collected by filtration, washed with MeOH, and dried to give 4-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride (5.0 g, 71%). 1H NMR (300 Hz, DMSO-d6) δ 8.12 (d, J=8.4 Hz, 2H), 7.91-7.96 (m, 3H), 7.58-7.66 (m, 1H), 7.31-7.53 (m, 1H), 7.27 (d, J=6.6, 1H), 6.97 (d, J=9.0, 1H), 2.43 (d, J=4.8 Hz, 3H). MS (ESI) m/z (M+H)+ 264.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741321B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-7349bd6e887b4576876388ab6d866fc3 |
| 出典メモ | uspto-grants-2010_06 |