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4,4'-Dimethylbenzhydrol → HCID 18319023、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,4'-Dimethylbenzhydrol | HCID 279356 | — |
| 反応物 | 4-[4-[2-(2-Hydroxyethylthio)ethoxy]phenyl]-1,1,1-trifluoro-2-butanone | HCID 18318995 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 18319023 | HCID 18319023 | 94.2% |
反応手順
A solution of 4-[4-[2-(2-hydroxyethylthio)ethoxy]phenyl]-1,1,1-trifluoro-2-butanone (1.20 g, 3.72 mmol), 4,4′-dimethylbenzhydrol (0.95 g, 4.47 mmol) and p-toluenesulfonic acid (0.035 g) in toluene (20 ml) was heated under reflux for 15 min. The cooled reaction mixture was diluted with ethyl acetate, washed with saturated sodium bicarbonate, brine and dried (magnesium sulfate). Evaporation of the solvent in vacuo and chromatography of the residue on silica gel (elution with a gradient of ethyl acetate 20-40% in hexane) gave 1.81 g (94%) of the title material as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06350892B1 |
| 出典データセット | uspto-grants-2002_02 |
| ORD ID | ord-efd51941c86345039b38f5193b571df7 |
| 出典メモ | uspto-grants-2002_02 |