反应详情

温度

55 °C

Borane methyl sulfide complex (2M in THF, 2.69 mL) was added dropwise to a solution of tert-butyl 2,2-difluoro-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate (example 37, step b) (0.55 g) in THF (15 mL). The reaction mixture was heated at 55° C. under nitrogen for 25 minutes and then cooled to room temperature. The mixture was quenched by careful dropwise addition of methanol (5 mL). N1,N2-dimethylethane-1,2-diamine (0.633 g) was then added and the mixture heated at 70° C. for minutes. The solvents were removed under reduced pressure and the residue was purified by flash silica chromatography using 4% methanol in dichloromethane with 1% triethylamine as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.32 g. Used directly.

1. temperaturecooled to room temperature
2. customThe mixture was quenched by careful dropwise addition of methanol (5 mL)
3. additionN1,N2-dimethylethane-1,2-diamine (0.633 g) was then added
4. temperaturethe mixture heated at 70° C. for minutes
5. customThe solvents were removed under reduced pressure
6. customthe residue was purified by flash silica chromatography
7. customPure fractions were evaporated to dryness