化工社化工社 化学情報印刷レポート · 研究参考用
4-Methyl-2,3,5,6-tetrafluorobenzyl alcohol → 2,3,5,6-tetrafluoro-4-methylbenzyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methyl-2,3,5,6-tetrafluorobenzyl alcohol | HCID 2734209 | — |
| 反応物 | ethyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate | HCID 14718703 | — |
| 触媒 | Titanium | HCID 23963 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,3,5,6-tetrafluoro-4-methylbenzyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate | HCID 14718864 | 46.6% |
反応手順
A mixture of ethyl (RS)-2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3,3-dimethylbutanoate (0.07 g), 2,3,5,6-tetrafluoro-4-methylbenzyl alcohol (0.1 g), titanium IV ethoxide (catalytic amount) and dry toluene (2 cm3) was heated at the reflux temperature for 10 hours. After cooling, the solvent was evaporated under reduced pressure to leave a brown gum, which was purified by preparative thin layer chromatography on 20 cm×20 cm×0.2 cm silica gel plates, eluting with dichloromethane containing 2% by volume ethyl acetate, to give the title compound (0.05 g) as an oil which solidified on standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04962109 |
| 出典データセット | uspto-grants-1990_10 |
| ORD ID | ord-491d0188b03a433490061091862b5c7e |
| 出典メモ | uspto-grants-1990_10 |