反应详情

温度

60 °C

A mixture of tert-butyl 5-oxa-2,8-diazaspiro[3.5]nonane-8-carboxylate (0.49 g) (example 176 step c), 2-(3-(2-bromoethyl)phenyl)ethanol (0.738 g) [Organometallics 2002, 21(20), 4217] and potassium carbonate (1.187 g) in acetonitrile (30 mL) and water (0.5 mL) was heated at 60° C. for 24 hours. The mixture was cooled to RT and filtered. The solvent was passed through a 10 g SCX cartridge and further acetonitrile then eluted through. The cartridge was then eluted with a 10% solution of 880 ammonia in acetonitrile (80 mL) to bring off product. The solvents were evaporated under reduced pressure and the residue was diluted with acetonitrile and then evaporated to dryness to afford the subtitled compound. Yield 0.610 g.

1. temperatureThe mixture was cooled to RT
2. filtrationfiltered
3. washthen eluted through
4. washThe cartridge was then eluted with a 10% solution of 880 ammonia in acetonitrile (80 mL)
5. customThe solvents were evaporated under reduced pressure
6. additionthe residue was diluted with acetonitrile
7. customevaporated to dryness