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Hydrogen Peroxide → 2-(3,5-Dichloro-1-oxido-pyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone | HCID 25005168 | — |
| 触媒 | Manganese dioxide | HCID 14801 | — |
| 触媒 | HCID 178477782 | HCID 178477782 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(3,5-Dichloro-1-oxido-pyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone | HCID 25005169 | — |
反応手順
To a solution of 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3′-oxetane]-6-yl}ethanone [121] (20.5 mg, 50 μmol) in CH2Cl2 (1 mL) was added 30% H2O2 (15 μL) and methyltrioxorhenium(VII) (5 mg). The mixture was stirred for 18 h, added MnO2 (5 mg) and was stirred for another hour. CH2Cl2 (10 mL) was added and the organic phase was washed with water. The combined organic phase was dried over MgSO4 and evaporated to dryness under reduced pressure. Standard HPLC purification afforded 14 mg of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08338431B2 |
| 出典データセット | uspto-grants-2012_12 |
| ORD ID | ord-0eb6c5e22bcb453e93177ccfb4df0523 |
| 出典メモ | uspto-grants-2012_12 |