反应详情

A mixture of benzyl ethyl(piperidin-4-yl)carbamate trifluoroacetate (4.14 mmol, 1.0 eq), 4-chloro-2,6-dimethylpyrimidine (0.706 g, 4.97 mmol, 1.2 eq) and K2CO3 (1.14 g, 8.28 mmol, 2.0 eq) in acetone (20 ml) was stirred for 14 hours at boiling temperature. After monitoring by TLC, the mixture was concentrated, diluted with DCM (200 ml), washed with water (80 ml) and sat. NaCl solution (80 ml), dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 2.0% MeOH in DCM). Yield: 63% (960 mg, 2.60 mmol)

1. concentrationthe mixture was concentrated
2. additiondiluted with DCM (200 ml)
3. washwashed with water (80 ml) and sat. NaCl solution (80 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by column chromatography (silica gel, 2.0% MeOH in DCM)