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Dimethylamine → 2-amino-5-bromo-N,N-dimethylpyridine-3-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-Amino-5-bromopyridine-3-sulfonyl chloride | HCID 53302026 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-amino-5-bromo-N,N-dimethylpyridine-3-sulfonamide | HCID 52335153 | 55% |
反応手順
To a cold (0 □C) suspension of 2-amino-5-bromo-3-pyridinesulfonyl chloride (92.1 mmol) in dry 1,4-dioxane (92 mL) was added pyridine (101.3 mmol) followed by a 2M solution of dimethylamine in THF (101.3 mmol). The reaction was allowed to warm to rt for 2 h, heated to 50 □C for 1 h, then cooled to rt. After standing for 2 h, the precipitate was collected by filtration and rinsed with a minimal amount of cold water. Drying the precipitate to constant weight under high vacuum provided 14.1 g (55%) of the title compound as a white solid. MS(ES)+ m/e 279.8, 282.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07592342B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-72e0a70fb94f4e948a2f3a21c488004b |
| 出典メモ | uspto-grants-2009_09 |