関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetamide | HCID 178 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 3-(2,6-dichloropyridin-4-yl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine | HCID 86649869 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 生成物 | N-(6-chloro-4-(1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)pyridin-2-yl)acetamide | HCID 87192560 | 25.2% |
反応手順
A mixture of Example 7a (1.44 g, 3.57 mmol), acetamide (0.295 g, 4.99 mmol), cesium carbonate (1.743 g, 5.35 mmol), palladium (II) acetate (0.024 g, 0.107 mmol), and Xantphos (0.093 g, 0.161 mmol) was degassed and heated at 85° C. in a sealed vial for 6 hours. The reaction mixture was cooled and concentrated. The residue was treated with 20% brine and extracted with EtOAc (2×). The organic layers were dried, concentrated, and purified on a 40 g column using the ISCO Companion flash system eluting with CH2Cl2/EtOAc (90:10) to give 0.384 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08435980B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-9cf9dd06848645bfa34fc70ecf343d49 |
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| 出典メモ | uspto-grants-2013_05 |
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