関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenol, 4-amino-2-fluoro- | HCID 2735918 | — |
| 反応物 | 1-acetyl-4,6-dichloro-3-methyl-1H-pyrrolo[2,3-b]pyridine | HCID 17979289 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Benzenamine,4-[(6-chloro-3-methyl-1h-pyrrolo[2,3-b]pyridin-4-yl)oxy]-3-fluoro- | HCID 17979286 | — |
反応手順
300 mg (1.16 mmol) of 1-acetyl-4,6-dichloro-3-methyl-1H-pyrrolo[2,3-b]pyridine (from example XL) and 320 mg (2.32 mmol) of powdered potassium carbonate are suspended in 9 ml of DMSO. The mixture is degassed, and 442 mg (3.48 mmol) of 4-amino-2-fluorophenol are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through CELITE (diatomaceous earth) and the filtercake is washed with ethyl acetate. The filtrate is extracted three times with sat. sodium bicarbonate solution and with sat. sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silica gel 60, mobile phase: DCM:methanol=50:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737153B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-f54b7a1f971e4a7496946caf6e8bee25 |
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| 出典メモ | uspto-grants-2010_06 |
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