化工社化工社 化学情報印刷レポート · 研究参考用
Citric Acid → 2-Bromo-1-[3-tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Phenyltrimethylammonium bromide dibromide | HCID 17977687 | — |
| 反応物 | 1-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone | HCID 58136808 | — |
| 溶媒 | MeOH tetrahydrofuran | HCID 21899815 | — |
| 生成物 | 2-Bromo-1-[3-tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone | HCID 58136782 | 292.5% |
反応手順
1-[3-tert-Butyl-5-(2-methoxyethoxy)phenyl]ethanone (O2.043; 1 g) was dissolved in methanol/THF (25 ml/25 ml), admixed with phenyltrimethylammonium tribromide (882 mg) while stirring and stirred at RT overnight. Then 50 ml of 20% citric acid solution were added and the mixture was stirred for 1 h. Subsequently, DCM (200 ml) was added and the mixture was extracted three times with DCM. Then the combined DCM phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min). 1.31 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198272B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-a25aebc613cf4db3876963c6003ed612 |
| 出典メモ | uspto-grants-2012_06 |