関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 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-Bromo-2-methoxy-5-nitropyridine | HCID 21584451 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Methoxy-3-morpholino-5-nitropyridine | HCID 68027925 | — |
反応手順
Morpholine (54 μl), cesium carbonate (336 mg), Pd2(dba)3 (57 mg), and Xantphos (72 mg) were added to a 1,4-dioxane (3 ml) solution containing 3-bromo-2-methoxy-5-nitropyridine (96 mg) in a nitrogen atmosphere, followed by stirring at 100° C. for 10 hours. The reaction solution was adjusted to room temperature, and water was added, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=4:1 to 2:1), and a yellow solid of 2-methoxy-3-morpholino-5-nitropyridine (54 mg) was thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08772320B2 |
|---|
| 出典データセット | uspto-grants-2014_07 |
|---|
| ORD ID | ord-f27689bc3ad54f79a56637174f7502b7 |
|---|
| 出典メモ | uspto-grants-2014_07 |
|---|
