関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 反応物 | Silanol, trimethyl-, 1,1'-sulfate | HCID 87573 | — |
| 反応物 | HCID 178418615 | HCID 178418615 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178418655 | HCID 178418655 | — |
反応手順
A solution of 3.0 g of trans-4-(4'-cyano-4-biphenylyl)cyclohexanol, 1.1 ml of 3,4-dihydro-2H-pyran in 30 ml of dichloromethane was treated at 0° C. with a solution of 0.007 g of bistrimethylsilyl sulfate in 2 ml of dichloromethane. The reaction mixture was stirred at 0° C. for a further 30 minutes and then washed once with sodium carbonate solution and twice with water and subsequently dried over magnesium sulfate, filtered and concentrated. The crude product was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9:1). Recrystallization from ethyl acetate at -20° C. gave 1.75 g of pure trans-4-(4'-cyano-4-biphenylyl)cyclohexyl tetrahydropyranyl ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05244597 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-5e5c25f893b444bd9bf8ae43f97a4d3f |
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| 出典メモ | uspto-grants-1993_09 |
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