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(3,4-dihydro-2H-pyran-2-yl)methyl 4-methylbenzene-1-sulfonate → Trans-6-[alpha-(4-chlorophenyl)-2,4-dichlorobenzyloxy]-2-tosyloxymethyltetrahydropyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (3,4-dihydro-2H-pyran-2-yl)methyl 4-methylbenzene-1-sulfonate | HCID 13071283 | — |
| 反応物 | 2,4,4'-Trichlorobenzhydrol | HCID 22565435 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 触媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | Trans-6-[alpha-(4-chlorophenyl)-2,4-dichlorobenzyloxy]-2-tosyloxymethyltetrahydropyran | HCID 53867744 | — |
反応手順
2.10 g of α-(4-chlorophenyl)-2,4-dichlorobenzyl alcohol and 1.78 of 2-tosyloxymethyl-3,4-dihydro-2H-pyran were dissolved in 40 ml of diethyl ester, and a catalytic amount (2 drops) of phosphorus oxytrichloride was added to the solution. The mixture was then stirred at room temperature for 4 days, after which 3 drops of triethylamine were added. The mixture was then concentrated by evaporation under reduced pressure and the residue was purified by column chromatography through silica gel eluted with a 15:5:1 by volume mixture of hexane, benzene and ethyl acetate, to give 3.41 g of the title compound in the form of a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04421758 |
| 出典データセット | uspto-grants-1983_12 |
| ORD ID | ord-b6aa40c21ef24b06a2d1e5d660883ff9 |
| 出典メモ | uspto-grants-1983_12 |