反应详情

A solution of (2-methylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate (example 4, step h) (0.408 g), 3-(bromomethyl)benzaldehyde (0.205 g) and triethylamine (0.36 mL) in acetonitrile (10 mL) was stirred at room temperature overnight. The solution was concentrated in vacuo and the residue partitioned between ethyl acetate and saturated sodium bicarbonate. The organic phase was washed twice with water, once with brine, then dried over anhydrous magnesium sulphate and purified by flash chromatography on silica eluted with 5% methanol in dichloromethane to afford the subtitled compound as a yellow gum. Yield 0.325 g.

1. concentrationThe solution was concentrated in vacuo
2. customthe residue partitioned between ethyl acetate and saturated sodium bicarbonate
3. washThe organic phase was washed twice with water, once with brine
4. dry with materialdried over anhydrous magnesium sulphate
5. custompurified by flash chromatography on silica
6. washeluted with 5% methanol in dichloromethane