反应详情

温度

0 °C

To a stirred solution of 0.9 g (2.2 mmol) {4-[2-(benzyloxy)ethoxy]-3-tert-butoxyphenyl}methanol and 976 mg (2.94 mmol) tetrabromo methane in 9 ml THF was added 775 mg (2.96 mmol) triphenylphosphin diluted in 4.5 ml THF at 0° C. dropwisly. The reaction mixture was stirred for 1 h at 0° C. The suspension was filtrated. The filter cake was washed with THF. The combined filtrates were concentrated in vacua. The crude product is purified by column chromatography (silica gel, hexane/ethylacetate gradient: 99:1→1:99). The desired product was obtained in 28% yield (313 mg, 0.76 mmol).

1. filtrationThe suspension was filtrated
2. washThe filter cake was washed with THF
3. concentrationThe combined filtrates were concentrated in vacua
4. customThe crude product is purified by column chromatography (silica gel, hexane/ethylacetate gradient: 99:1→1:99)