化工社化工社 化学情報印刷レポート · 研究参考用
Methyl iodide → 4-Bromo-2-butyl-6-fluoro-5-methoxy-1-indanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Bromo-2-butyl-6-fluoro-5-hydroxy-1-indanone | HCID 21990852 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Bromo-2-butyl-6-fluoro-5-methoxy-1-indanone | HCID 21990906 | 81.6% |
反応手順
A mixture of 4-bromo-2-butyl-6-fluoro-5-hydroxy-1-indanone (2.17 g, 7.23 mmol), N,N-dimethylformamide (14.5 mL), methyl iodide (0.675 mL, 10.84 mmol), and sodium bicarbonate (1.50 g, 18.1 mmol) was stirred at room temperature for 17 hours. The solvent was evaporated under vacuum. The residue in EtOAc (150 mL) was washed with water (5×100 mL) and brine (50 mL), dried over MgSO4, filtered, and evaporated under vacuum to an oil (2.29 g). The crude product was dissolved in CH2CL2 (5 mL) and the solution filtered through a pad of EM silica gel 60 (20 mL) using an additional 60 mL of CH2Cl2 to elute the silica gel. The CH2Cl2 filtrate was evaporated under vacuum to afford 4-bromo-2-butyl-6-fluoro-5-methoxy-1-indanone (1.86 g) as a pink oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087599B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-835f01ea929a484fbdde0611e5ce74b3 |
| 出典メモ | uspto-grants-2006_08 |