反应详情

温度

60 °C

To a mixture of 4-fluoro-3-(3-hydroxypropyl)phenol (1.5 g), methyl (2R)-2-chloropropanoate (1.30 g) in DMSO (7.5 mL) was added Cs2CO3 (3.45 g) at ambient temperature. The mixture was stirred at 60° C. for 3 hours. After cooling to ambient temperature, the reaction mixture was diluted with EtOAc (50 mL) and washed successively with water (30 mL) two times and brine (30 mL). The organic layer was dried over anhydrous MgSO4, filtered and evaporated in vacuo to give crude oil. The crude oil was purified by silica gel column chromatography (n-hexane:EtOAc=4:1-2:1) to give methyl(2S)-2-[4-fluoro-3-(3-hydroxypropyl)phenoxy]propanoate (1.51 g) as a colorless oil.

1. temperatureAfter cooling to ambient temperature
2. washwashed successively with water (30 mL) two times and brine (30 mL)
3. dry with materialThe organic layer was dried over anhydrous MgSO4
4. filtrationfiltered
5. customevaporated in vacuo
6. customto give crude oil
7. customThe crude oil was purified by silica gel column chromatography (n-hexane:EtOAc=4:1-2:1)