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Boron tribromide → Awd 12-281
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide | HCID 11123551 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Awd 12-281 | HCID 6918428 | — |
反応手順
1.4 g of N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide (3 mmol) is dissolved in 100 ml of dichloromethane. The solution is heated to reflux and treated with a solution of 14 mmol of BBr3 in 15 ml of dichloromethane with stirring. The reaction mixture is refluxed for 3 hours. After cooling, the solution is intensively stirred for 3 hours at 20° C. with 200 ml of an aqueous sodium hydrogencarbonate solution. The product crystallizes out, it is isolated, dried at 60° C. and recrystallized from 80 ml of ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06602890B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-efc4e913385047dba51015f9b7803f11 |
| 出典メモ | uspto-grants-2003_08 |