反应详情

A solution of 3,3-difluoropyrrolidine (215 mg, 1.5 mmol), 4,6-dichloro-pyrimidine (223 mg, 1.5 mmol) and DIPEA (194 mg, 1.5 mmol) in 1,4-dioxane (3.0 mL) was heated at 100° C. for 16 hours. The reaction was cooled to room temperature and then partitioned between EtOAc and water. The organic phase was separated and washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated. The residue was separated with flash chromatography (25+S Biotage, 20% EtOAc/pentane) to afford 160 mg (48.6%) of 4-chloro-6-(3,3-difluoropyrrolidin-1-yl)pyrimidine as a solid.

1. custompartitioned between EtOAc and water
2. customThe organic phase was separated
3. washwashed with saturated sodium chloride solution
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was separated with flash chromatography (25+S Biotage, 20% EtOAc/pentane)