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m-Chloroperbenzoic acid → 3-[8-(2,6-difluorophenyl)-2-(methylsulfinyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide | HCID 11950263 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-[8-(2,6-difluorophenyl)-2-(methylsulfinyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide | HCID 11950264 | 77% |
反応手順
To a solution of 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (600 mg, 1.24 mmol) in CH2Cl2 (15 mL) was added m-CPBA (293 mg, 1.31 mmol). The mixture was stirred at room temperature for 10 minutes, then directly loaded onto a column. CombiFlash chromatography (mobile phase EtOAc/Hexane) afforded the title compound as a white solid 475 mg (77%). LC-MS m/z 500 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07674789B2 |
| 出典データセット | uspto-grants-2010_03 |
| ORD ID | ord-5df77290805243729f56bfbd482a1429 |
| 出典メモ | uspto-grants-2010_03 |