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Water → 2-Amino-3-nitro-5-pyridin-3-yl-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Amino-5-bromo-3-nitropyridine | HCID 138878 | — |
| 反応物 | 3-Pyridinylboronic acid | HCID 2734378 | — |
| 触媒 | Dichlorobis(tricyclohexylphosphine)pallium (II) | HCID 11050900 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Amino-3-nitro-5-pyridin-3-yl-pyridine | HCID 21882712 | — |
反応手順
0.21 g of dichlorobis(tricyclohexylphosphine)palladium, 0.66 g of 3-pyridyl-boronic acid and 14 ml of a 2N sodium carbonate solution are added to a solution of 1.02 g of 2-amino-5-bromo-3-nitropyridine in 40 ml of degassed dioxane. The mixture is heated to reflux under N2 for 28 hours and, after cooling and addition of water, extracted three times with dichloromethane. The combined organic phases are dried over sodium sulfate, concentrated and the residue is crystallized from ethyl acetate. This gives 0.58 g of the title compound of m.p. 226–228° C. The mass spectrum shows the molecular peak MH+ at 217.2 Da.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138399B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-a9fbc260b4fa49dfacc3a3a1be196a4f |
| 出典メモ | uspto-grants-2006_11 |