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Sodium periodate → 6,7-Dihydro[1,4]oxathiino[2,3-c]pyridazine-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium periodate | HCID 23667635 | — |
| 反応物 | 3-Ethenyl-6,7-dihydro[1,4]oxathiino[2,3-c]pyridazine | HCID 67526496 | — |
| 触媒 | Osmium Tetroxide | HCID 30318 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 6,7-Dihydro[1,4]oxathiino[2,3-c]pyridazine-3-carbaldehyde | HCID 71504254 | 36% |
反応手順
A solution of 3-ethenyl-6,7-dihydro[1,4]oxathiino[2,3-c]pyridazine (320 mg) in 1,4-dioxane/water (20 ml/5 ml) was treated with an aqueous solution of osmium tetroxide (4% w/v, 2 ml) and sodium periodate (1.08 g), initially stirred in an ice-bath, then allowed to warm to room temperature. After 2.5 hours the mixture was evaporated to dryness and dissolved in 1,4-dioxane and chloroform. Silica gel was added and the mixture was evaporated to dryness, added to a silica column (50 g) and chromatographed, eluting with 0-100% ethyl acetate in hexane, to afford a white solid (116 mg, 36%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07709483B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-75ac3cc0815e48259e98725a1f063b5d |
| 出典メモ | uspto-grants-2010_05 |