関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methyl-5-Nitroaniline | HCID 7444 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,4-Dichloropyridine | HCID 33515 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-[(4-Chloro)pyridin-2-ylamino]-1-methyl-4-nitrobenzene | HCID 68693745 | 34.2% |
反応手順
To 2.00 g of 2,4-dichloropyridine, 2.26 g of 2-methyl-5-nitroaniline, 121 mg of palladium (II) acetate, 336 mg of (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl [(±)-BINAP] and 6.16 g of cesium carbonate, 120 ml of toluene was added, and then the mixture was stirred with heating at 70° C. for 23 hours under an argon atmosphere. After insolubles were removed by filtration, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain a crude product. The crude product was washed with diethyl ether to obtain 1.22 g of the objective compound as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07728131B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-d685328ebf2549899ea59d9ce7212bdc |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|