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4-Toluenesulfonyl chloride → 4-bromo-7-methoxy-1-tosyl-1H-pyrrolo[2,3-c]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-bromo-7-methoxy-1H-pyrrolo[2,3-c]pyridine | HCID 11806401 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-bromo-7-methoxy-1-tosyl-1H-pyrrolo[2,3-c]pyridine | HCID 89657546 | 100% |
反応手順
A solution of Example 1b (7.42 g, 32.7 mmol) in dimethylformamide (235 mL) was stirred at room temperature. To this solution was added sodium hydride (1.18 g, 1.96 g of 60% dispersion in oil, 49.0 mmol), and the reaction mixture was stirred for 10 min. P-toluenesulfonyl chloride (9.35 g, 49.0 mmol) was then added portion-wise, and the mixture was stirred at room temperature under nitrogen for 16 hours. The reaction mixture was quenched carefully with water and the resulting beige solid collected by vacuum filtration on a Buchner funnel, and washed with water. The solid was collected and dried in a vacuum oven at 50° C. to provide 12.4 g (100%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09296741B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-5728ee9f8abc41cbbb4db3798db6aed7 |
| 出典メモ | uspto-grants-2016_03 |