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Ozone → (+/-)-cis-6-(2-Oxoethyl)-2,2-dimethyl-1,3-dioxane-4-acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ozone | HCID 24823 | — |
| 反応物 | (+/-)-cis-2,2-Dimethyl-6-(2-propenyl)-1,3-dioxane-4-acetonitrile | HCID 15045109 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (+/-)-cis-6-(2-Oxoethyl)-2,2-dimethyl-1,3-dioxane-4-acetonitrile | HCID 86744690 | — |
反応手順
A solution of (±)-cis-2,2-dimethyl-6-(2-propenyl)-1,3-dioxane-4-acetonitrile, 3 g (15.36 mmol), in 100 mL of dichloromethane is cooled to -78° C. under nitrogen. Ozone (Welsbach generator, flow rate 0.1, voltage=90 V) is then passed through a fritted gas inlet tube into the solution until the blue color of ozone appears. The current is turned off, and oxygen bubbled through until the blue color is discharged. Triphenylphosphine, 4.2 g (16 mmol), is added and the colorless solution allowed to warm to room temperature. Flash chromatography provides, after concentration in vacuo, 2.5 g of pure (±)-cis-6-(2-oxoethyl)-2,2-dimethyl-1,3-dioxane-4-acetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05097045 |
| 出典データセット | uspto-grants-1992_03 |
| ORD ID | ord-0c8aad2dd6b941fc83eec9a2ff44f2ed |
| 出典メモ | uspto-grants-1992_03 |