反应详情

A solution of 3-(3-formylphenoxy)propyl methanesulfonate (example 95, step a) (0.209 g) and (2-methylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate (example 4, step h) (0.32 g) and triethylamine (0.282 mL) in acetonitrile (10 mL) were heated at 65° C. for 18 hours. The solvent was evaporated off under reduced pressure and the residue partitioned between ethyl acetate and brine. The organic layer was dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography using 2% methanol and 1% triethylamine in dichloromethane. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.157 g.

1. customThe solvent was evaporated off under reduced pressure
2. customthe residue partitioned between ethyl acetate and brine
3. dry with materialThe organic layer was dried over sodium sulphate
4. filtrationfiltered
5. customthe solvent evaporated under reduced pressure
6. customThe crude product was purified by flash silica chromatography
7. customPure fractions were evaporated to dryness