反应详情

温度

80 °C

A mixture of intermediate (5) (0.114 mol), 1-(2-bromoethyl)-4-methoxy-benzene (0.172 mol) and K2CO3 (0.219 mol) in ACN (200 ml) was stirred at 80° C. for 2 hours. Water was added and the mixture was extracted with DCM. The organic layer was separated, dried , filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 95/5/0.2). The pure fractions were collected and the solvent was evaporated, yielding 28.5 g of 8-[2-(4-methoxyphenyl)ethyl]-1,4-dioxa-8-azaspiro[4.6]undecane (intermediate 6).

1. extractionthe mixture was extracted with DCM
2. customThe organic layer was separated
3. customdried
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 95/5/0.2)
7. customThe pure fractions were collected
8. customthe solvent was evaporated