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Ethyl Acetate → 2-Bromo-4-isopropylanisole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ammonium nitrate | HCID 22985 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4-Isopropylanisole | HCID 77783 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Bromo-4-isopropylanisole | HCID 22087678 | 99.7% |
反応手順
A solution of 20.0 g of 1-isopropyl-4-methoxy benzene, 1.07 g of ammonium nitrate, and 23.7 g of N-bromosuccinimide in MeCN (66.5 ml) was stirred at room temperature for one hour. To the reaction solution was added EtOAc and a saturated aqueous solution of NaHCO3, liquid separation was performed, and the aqueous layer was extracted with EtOAc. The combined organic layer was washed with saturated brine and dried over MgSO4, then, the drying agent was separated by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silicagel 60; mobile phase: EtOAc/n-hexane=1/9, v/v) to obtain 30.4 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08030499B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-8464590027054288acd4b369abbbbe2c |
| 出典メモ | uspto-grants-2011_10 |