反应详情

温度

50 °C

1-(3,5-Dihydroxyphenyl)ethanone (1.0 g) and ethyl bromide (0.531 ml) were dissolved at RT in DMF (20 ml), and sodium hydride (189 mg) was added. After stirring at 50° C. for 2 h, cyclohexylmethyl bromide (1.36 ml) was added, followed by further sodium hydride (315 mg). After stirring at 50° C. for another 2 h, the DMF was drawn off and the residue was taken up in EA, washed with water, dried, filtered and concentrated. The residue was purified using silica gel (80 g cartridge, n-heptane/EA gradient of 0-20% within 60 min). 378 mg of the title compound were obtained. LC-MS rt: 2.07 min [M+H]+: 277.2 (met. a)

1. stirringAfter stirring at 50° C. for another 2 h
2. washwashed with water
3. customdried
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified
7. customsilica gel (80 g cartridge, n-heptane/EA gradient of 0-20% within 60 min)