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m-Chloroperbenzoic acid → N-[3-(1,1,2,2-tetrafluoroethoxy)phenyl]-4-(N-oxido-4-pyridyl)-2-pyrimidine-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | (4-Pyridin-4-yl-pyrimidin-2-yl)-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-amine | HCID 9799152 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[3-(1,1,2,2-tetrafluoroethoxy)phenyl]-4-(N-oxido-4-pyridyl)-2-pyrimidine-amine | HCID 19966995 | — |
反応手順
500 mg (1.37 mmol)of N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4(4-pyridyl)-2-pyrimidineamine are suspended in 10 ml of methylene chloride; 430 mg (1.37 mmol) of m-chloroperbenzoic acid are added and the reaction mixture is stirred for 4 h at RT. After extraction with water and 2N aqueous sodium hydroxide solution, the organic phase is dried and concentrated using a rotovapor. Chromatography (methylene chloride/methanol=19:1 to 9:1) and subsequent crystallisation (methylene chloride/diethyl ether) give N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(N-oxido-4-pyridyl)-2-pyrimidineamine in the form of lemon-yellow crystals; FAB-MS: 381 (M+ +H), m.p. 191°-192°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05612340 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-475597d72bb04a2e97a8d0419d8fdb6c |
| 出典メモ | uspto-grants-1997_03 |