反应详情

4-Chloro-2-(trifluoromethyl)pyrimidine (2.72 mmol, 1 eq.) and isopropanol (4 ml) were introduced into a microwave vessel. tert-Butyl 2,8-diazaspiro[4.5]decane-2-carboxylate (2.72 mmol, 1 eq.) and DIPEA (0.6 ml, 6.8 mmol), 2.5 eq.) were added in succession and the reaction mixture was introduced into a microwave oven at 75° C. for 45 min. After TLC control, the reaction mixture was concentrated on a rotary evaporator. A reddish liquid remained and was diluted with methylene chloride (200 ml). The organic phase was washed with water (2×100 ml) and sat. NaCl solution (50 ml), dried over sodium sulfate and concentrated. The brown liquid residue was purified by column chromatography (silica gel, ethyl acetate). Yield: 47%

1. additionthe reaction mixture was introduced into a microwave oven at 75° C. for 45 min
2. concentrationAfter TLC control, the reaction mixture was concentrated on a rotary evaporator
3. additionwas diluted with methylene chloride (200 ml)
4. washThe organic phase was washed with water (2×100 ml) and sat. NaCl solution (50 ml)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe brown liquid residue was purified by column chromatography (silica gel, ethyl acetate)