反应详情

5 g of 2,2-bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propoxy]phenyl}propane were heated at 100°-110° C. in 100 ml of acetic anhydride, with stirring, for 6 hours. After completion of the reaction, the reaction mixture was condensed by evaporation under reduced pressure and then 150 ml of benzene were added to dissolve the residue. The benzene solution was washed successively with a 2% w/w sodium carbonate solution and water. The solvent was then removed and the residue was purified by column chromatography through silica gel eluted with a 8:1:1:1 by volume mixture of ethyl acetate, benzene, ethanol, and triethylamine. The desired Compound No. 68 was obtained in the form of white crystals, melting point 147°-149° C.

1. customAfter completion of the reaction
2. customcondensed
3. customby evaporation under reduced pressure
4. addition150 ml of benzene were added
5. dissolutionto dissolve the residue
6. washThe benzene solution was washed successively with a 2% w/w sodium carbonate solution and water
7. customThe solvent was then removed
8. customthe residue was purified by column chromatography through silica gel
9. washeluted with a 8:1:1:1 by volume mixture of ethyl acetate, benzene, ethanol, and triethylamine
10. custom68 was obtained in the form of white crystals, melting point 147°-149° C.