反応 #353383

反応方程式

ethyl ether

Cyclopentyl bromide

phenol

potassium carbonate

cyclopentyl bromide

potassium carbonate

→

product

収率 98.0%

3-Cyclopentyloxy-4-methoxybromobenzene

収率 98.0%

溶媒

acetonitrile

hexane

反応条件

後処理

1. 1
   温度at reflux temperature
2. 2
   その他the reaction (1 hour)
3. 3
   その他Reaction progress
4. 4
   ろ過The suspension was filtered
5. 5
   洗浄The filtered material was washed with ethyl acetate (2×100 mL)
6. 6
   濃縮concentrated
7. 7
   workup.DISTILLATIONdistilled under vacuum (0.1 mm, 140° C.°145° C.)

実験手順

Cyclopentyl bromide (37 mL, 0.345 mol) was added to a slurry of the phenol (50 g, 0.246 mol) and potassium carbonate (17 g, 0.123 mol) in acetonitrile (500 mL) at reflux temperature. After two hours, cyclopentyl bromide (13.2 mL, 0.123 mol) and potassium carbonate (8.5 g, 0.062 mol) were added to complete the reaction (1 hour). Reaction progress was monitored by TLC (50% ethyl ether in hexane). The suspension was filtered. The filtered material was washed with ethyl acetate (2×100 mL). The filtrates were combined, concentrated and distilled under vacuum (0.1 mm, 140° C.°145° C.) to yield 65.62 g (0.242 mol, 98%) of product,

出典