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Methanol → 7-Bromofuro[3,2-c]pyridin-4(5H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4H,5H-furo(3,2-c)pyridin-4-one | HCID 288746 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7-Bromofuro[3,2-c]pyridin-4(5H)-one | HCID 17985527 | — |
反応手順
Add N-bromosuccinimide (63.16 g, 354.9 mmol) as a solution in anhydrous acetonitrile (480 mL) to a suspension of 5H-furo[3,2-c]pyridin-4-one (36.9 g, 273 mmol) in anhydrous acetonitrile (740 mL) at 0° C. over 1 hour. Warm to room temperature, add anhydrous methyl alcohol (1.5 L) and stir at room temperature for 18 hours. Quench with water (20 ml) and saturated sodium bicarbonate (20 mL), concentrate to a volume of 1.3 liters, and pour into water (1.3 L). Collection of the precipitate by filtration and drying (vacuum oven 2 days 40-60° C.) gives the title compound as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08058425B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-9bd1f2e713f14c15b1a56ea1de3a101f |
| 出典メモ | uspto-grants-2011_11 |