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Triphenylphosphine → 5-methyl-3-{3-[5-(4-methylpiperazin-1-yl)pyrimidin-2-yl]benzyl}-3H-oxazolo[4,5-b]pyridin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Di-tert-butyl azodicarboxylate | HCID 97268 | — |
| 反応物 | 5-Methyloxazolo[4,5-b]pyridin-2(3H)-one | HCID 10012075 | — |
| 反応物 | {3-[5-(4-Methylpiperazin-1-yl)pyrimidin-2-yl]phenyl}methanol | HCID 59484860 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-methyl-3-{3-[5-(4-methylpiperazin-1-yl)pyrimidin-2-yl]benzyl}-3H-oxazolo[4,5-b]pyridin-2-one | HCID 58486104 | — |
反応手順
67 mg (0.44 mmol) of 5-methyl-3H-oxazolo[4,5-b]pyridin-2-one and 125 mg (0.44 mmol) of {3-[5-(4-methylpiperazin-1-yl)pyrimidin-2-yl]phenyl}methanol are suspended in 5 ml of DMF with 222 mg (0.67 mmol) of polymer-bound triphenylphosphine (about 3 mmol of triphenylphosphine per g), and the mixture is shaken at room temperature for 30 min. 156 mg (0.67 mmol) of di-tert-butyl azodicarboxylate are added. The reaction mixture is shaken at room temperature for 15 h. The reaction mixture is filtered, the residue is evaporated, and the residue is purified by column chromatography on silica gel, giving 67 mg of “A125”; HPLC: Rt=2.26 min (method B); ESI: 418 (M+H);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08071593B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-51384a395767447e990e66c19e294b6d |
| 出典メモ | uspto-grants-2011_12 |