化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → HCID 178418683、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Silanol, trimethyl-, 1,1'-sulfate | HCID 87573 | — |
| 反応物 | HCID 178418673 | HCID 178418673 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178418683 | HCID 178418683 | 50.6% |
反応手順
A solution of 1.2 g of trans-4-(4'-decyl-4-biphenylyl)cyclohexyl tetrahydropyranyl ether in 40 ml of methanol and 2 ml of diethyl ether was treated with a solution of 7.3 mg of bistrimethylsilyl sulfate in 2 ml of dichloromethane. The reaction mixture was stirred at room temperature for 2 hours and then treated with 0.2 ml of pyridine. Subseguently, the reaction mixture was concentrated and the residue was then taken up in 50 ml of dichloromethane, washed twice with water, dried over magnesium sulfate, filtered and again concentrated. The residue was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9:1). Recrystallization from methanol gave 0.5 g of trans-4-(4'-decyl-4-biphenylyl)cyclohexanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05244597 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-5644e5fd1d534b5297d22337a4455595 |
| 出典メモ | uspto-grants-1993_09 |