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p-Toluenesulfonic acid → 2-Propanone, 1,3-bis[(tetrahydro-2H-pyran-2-yl)oxy]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 反応物 | Dihydroxyacetone dimer | HCID 4180364 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2-Propanone, 1,3-bis[(tetrahydro-2H-pyran-2-yl)oxy]- | HCID 11010660 | — |
反応手順
9.0 g of dihydroxyacetone dimer, 21.0 g of 3,4-dihydro-2H-pyran and a catalytic amount of p-toluenesulfonic acid were added to 70 ml of dichloromethane and stirred under ice-cooling for 3 hours. After the completion of the reaction, 150 ml of diethyl ether was added thereto. The mixture was then washed with a saturated aqueous solution of sodium hydrogencarbonate and dried over anhydrous magnesium sulfate. After distilling off the solvent, the oily residue thus obtained was subjected to chromatography wherein silica gel was employed as a carrier while hexane/ethyl acetate was employed as a mobile phase. Thus 16.5 g of 1,3-bis(2-tetrahydro-pyranyloxy)propan-2-one was obtained as a colorless viscous liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05102895 |
| 出典データセット | uspto-grants-1992_04 |
| ORD ID | ord-b2dbd7a34dee46b58b73467fbbc6c501 |
| 出典メモ | uspto-grants-1992_04 |