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 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4,6-Dichloropyrimidine | HCID 70943 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-[(6-Chloro)pyrimidin-4-ylamino]-1-methyl-4-nitrobenzene | HCID 86061071 | 78.6% |
反応手順
2.64 g of 2-methyl-5-nitroaniline and 10.33 g of 4,6-dichloropyrimidine were stirred with heating at 110° C. for 16 hours. After air cooling, the reaction solution was dissolved in methanol. An aqueous saturated sodium hydrogen carbonate solution and ethyl acetate were added to separate the aqueous layer. The aqueous layer was further subjected to extraction with ethyl acetate twice. The organic layers were combined and dried over anhydrous magnesium sulfate, and then 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 diisopropyl ether to obtain 3.61 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-64102c395d4244efb41b9d6bfcb88a88 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|