反应详情

温度

75 °C

A mixture of 2-chloro-4-(hydroxymethyl)-5-methoxyphenol (intermediate 54; 0.5 g, 2.61 mmol), 1,3-dibromopropane (1.61 ml; 15.71 mmol) and potassium carbonate (737 mg; 5.23 mmol) in 12 ml acetone was heated to 75° C. in a sealed vessel and stirred for 16 hr. The solids were filtered and washed with acetone and the combined filtrates were concentrated to dryness and purified by preparative reversed-phase HPLC (hexane/EtOAc from 0 to 40%), affording the title compound (80%) as a light yellow oil.

1. filtrationThe solids were filtered
2. washwashed with acetone
3. concentrationthe combined filtrates were concentrated to dryness
4. custompurified by preparative reversed-phase HPLC (hexane/EtOAc from 0 to 40%)