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Dichloromethane → 5-Nitro-3-phenylpyridin-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Phenylboronic Acid | HCID 66827 | — |
| 反応物 | HCID 178526840 | HCID 178526840 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 5-Nitro-3-phenylpyridin-2-ol | HCID 178526835 | — |
反応手順
In a schlenck tube, a mixture of 3-iodo-5-nitropyridin-2-ol (7.52 mmol, 2 g), phenylboronic acid (8.28 mmol, 1.01 g), PdCl2dppf.DCM (0.75 mmol, 0.6 g), Cs2CO3 (22.56 mmol, 7.4 g) in a dioxane/water 4:1 mixture (26 ml) was heated at 100° C. for 4 hours, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The organic phase was evaporated and the crude was suspended in methanol affording a solid that was filtered off and dried under vacuum overnight affording 1.2 g (74% of yield) of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536165B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-c87b15bf4ba24b01a04e01ed10774af2 |
| 出典メモ | uspto-grants-2013_09 |