反应详情

温度

20 °C

A solution of (2-methylthiazol-4-yl)(7-oxa-3,10-diazaspiro[5.6]dodecan-10-yl)methanone trifluoroacetate (example 89, step g) (0.21 g) in acetonitrile (15 mL) was treated with triethylamine (0.214 mL) followed by 2-(3-(bromomethyl)phenyl)ethanol (example 6, step a) (0.121 g). The reaction mixture was stirred for 3 hours at 20° C. The solvent was evaporated under reduced pressure and the residue was partitioned between DCM and saturated sodium bicarbonate solution. The aqueous layer was re-extracted twice with DCM and the combined organics were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. The crude product was purified by flash silica chromatography using 6% methanol in dichloromethane with 1% triethylamine as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.21 g.

1. customThe solvent was evaporated under reduced pressure
2. customthe residue was partitioned between DCM and saturated sodium bicarbonate solution
3. extractionThe aqueous layer was re-extracted twice with DCM
4. dry with materialthe combined organics were dried over sodium sulphate
5. filtrationfiltered
6. customthe solvent removed under reduced pressure
7. customThe crude product was purified by flash silica chromatography
8. customPure fractions were evaporated to dryness