関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-tert-Butyl-4-methylphenol | HCID 17004 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 178426895 | HCID 178426895 | — |
反応手順
In an atmosphere of nitrogen, 16.42 g (100 mmol) of 2-tert-butyl-4-methylphenol was dissolved in 100 ml of diethyl ether and 33.3 ml of methylmagnesium bromide (100 mmol of diethyl ether solution) was added dropwise to this at 0° C. taking 5 minutes. After completion of the dropwise addition, the mixture was stirred at 25° C. for 10 minutes. After that, the diethyl ether was evaporated under vacuum, and 150 ml of toluene was added to obtain a toluene solution of 2-tert-butyl-4-methylphenoxymagnesium bromide. To the solution, 5.61 g (50 mmol) of 2-thiophenecarboxyaldehyde was added dropwise at 25° C. After stirring for 24 hours, 5% aqueous hydrochloric acid solution was added and aqueous layer was separated. After the organic layer was washed with a saturated aqueous sodium chloride solution, it was dried with anhydrous magnesium sulfate and the solvent was removed by evaporation. The residue was purified by a silica gel column chromatography (a developing solvent: hexane/ethyl acetate=30/1) to obtain 2-bis(2-hydroxy-3-tert-butyl-5-methylphenyl)methylthiophene in a yield of 63%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05840646 |
|---|
| 出典データセット | uspto-grants-1998_11 |
|---|
| ORD ID | ord-652e5f4fcaae48c0957b2b8d7ad406e5 |
|---|
| 出典メモ | uspto-grants-1998_11 |
|---|