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Bromine → 4-(3-Bromo-1-benzothiophen-2-yl)-2-methylsulfonylpyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 4-(Benzo[b]thiophen-2-yl)-2-(methylsulfonyl)pyrimidine | HCID 57428827 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-(3-Bromo-1-benzothiophen-2-yl)-2-methylsulfonylpyrimidine | HCID 60204304 | 80.6% |
反応手順
Bromine (0.48 g, 3.02 mmol) was slowly added at rt to a mixture of 4-(benzo[b]thiophen-2-yl)-2-(methylsulfonyl)pyrimidine (0.73 g, 2.52 mmol) in acetic acid (20 mL). The resulting mixture was stirred at rt for 15 h and then heated at 60° C. for 5 h. After cooling to rt, acetic acid was removed in vacuo. 100 mL of saturated sodium bicarbonate was added and the mixture was extracted with dichloromethane (3×100 mL).). The combined organic layer was washed with brine (200 mL), dried over anhydrous sodium sulfate and filtered. The solvent was evaporated in vacuo and the solid treated with 20 mL of methanol, filtered and dried to give the title compound (0.75 g, 80%). MS (M+H)+ 369/371.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07858785B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-0bad9435eb1f4f398edd48f3cf1a346b |
| 出典メモ | uspto-grants-2010_12 |