反应详情

A solution of 0.75 g of 6-azaspiro[2.5]octane trifluoroacetate (3.30 mmol, 1 eq.) and 0.75 ml of DIPEA (1.3 eq.) in 6 ml of dichloroethane was added under argon to a solution of 0.65 g of methyl (S)-4,4-difluoro-2-isocyanatopentanoate (3.36 mmol) in 4 ml of dichloroethane. The reaction mixture was stirred at RT overnight. The mixture was diluted with 10 ml of dichloromethane and washed with saturated NaHCO3 solution. The organic phase was dried over MgSO4 and then concentrated under reduced pressure. The residue thus obtained was purified by preparative HPLC (gradient: acetonitrile/water and addition of 0.05% TFA. The product-containing fractions were combined and freeze-dried.

1. washwashed with saturated NaHCO3 solution
2. dry with materialThe organic phase was dried over MgSO4
3. concentrationconcentrated under reduced pressure
4. customThe residue thus obtained
5. customwas purified by preparative HPLC (gradient
6. additionacetonitrile/water and addition of 0.05% TFA
7. customfreeze-dried