反应详情

温度

85 °C

To a stirred solution of 4-(1-(4-(2-Chloroethoxy)phenyl)-1-(4-hydroxyphenyl)-but-1-en-2-yl)-2-methoxyphenol (88 mg, impure) in 10 mL MeOH was added 2 mL CH3NH2 (aq). After the mixture was heated at 85° C. for 24 h., the solvent was removed in vacuo, EtOAc was added, the mixture was washed with water and brine, dried over Na2SO4, filtered and the filtrate was evaporated in vacuo. The residue was purified by column chromatography (CH2Cl2/MeOH(NH3 gas)=10/1) to give the desired product (42 mg, 48% yield, Z/E=1/1) as a white solid. m/z=420[M+1]+.

1. customthe solvent was removed in vacuo, EtOAc
2. additionwas added
3. washthe mixture was washed with water and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customthe filtrate was evaporated in vacuo
7. customThe residue was purified by column chromatography (CH2Cl2/MeOH(NH3 gas)=10/1)