反应详情

温度

90 °C

561 mg (2.8 mmol) of tert-butyl 3-aminopiperidine-1-carboxylate, 700 mg (2.16 mmol) of tert-butyl [6-chloro-3-(trifluoroacetyl)pyridin-2-yl]carbamate (Example 7A) and 0.56 ml (3.23 mmol) of diisopropylethylamine were suspended in 14 ml of DMSO and heated to 90° C. in a microwave reactor for 45 min. The reaction mixture was diluted with ethyl acetate (100 ml) and washed with saturated aqueous ammonium chloride solution (3×40 ml) and then with saturated aqueous sodium hydrogencarbonate solution (40 ml). The organic phase was dried over magnesium sulphate and concentrated. The residue was chromatographed on silica gel (eluent: cyclohexane/ethyl acetate 5:1 to 1:1). 670 mg (63% of theory) of the product were isolated.

1. washwashed with saturated aqueous ammonium chloride solution (3×40 ml)
2. dry with materialThe organic phase was dried over magnesium sulphate
3. concentrationconcentrated
4. customThe residue was chromatographed on silica gel (eluent: cyclohexane/ethyl acetate 5:1 to 1:1)
5. custom670 mg (63% of theory) of the product were isolated