반응 #1563943
ord-a7adbb57ebae4983837159bbc90c1b01
반응 방정식
용매
반응 조건
온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The reaction mixture was quenched with 1M aq
- 2추출NaOH solution, extracted with diethyl ether (3×100 mL)
- 3건조dried over anhydrous sodium sulphate
- 4농축concentrated under reduced pressure
- 5기타to afford the crude, which
- 6기타was purified by column chromatography (using silica gel and 2% ethyl acetate in hexane as eluent)
실험 절차
1-bromo-2-methoxyethane (5.49 g, 39.5 mmol) was added to a mixture of 2-bromo-4-fluoro phenol (5 g, 26.18 mmol) and K2CO3 (11.5 g, 83.25 mmol) in CH3CN (41.5 mL) and continued stirring at 80° C. for 16 hr. The reaction mixture was quenched with 1M aq.NaOH solution, extracted with diethyl ether (3×100 mL), dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford the crude, which was purified by column chromatography (using silica gel and 2% ethyl acetate in hexane as eluent) to afford the desired compound (Int-42). 1H NMR (300 MHz, CDCl3) δ ppm 7.3 (1H, m), 6.9 (1H, m), 6.7 (1H, m), 4.1 (2H, t), 3.8 (2H, t), 3.5 (3H, s).