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 11A) and 0.56 ml (3.23 mmol) of diisopropylethylamine were suspended in 14 ml of DMSO and heated in a microwave reactor at 90° C. 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 bicarbonate solution (40 ml), and the organic phase was dried over magnesium sulfate, diluted and concentrated. The residue was chromatographed on silica gel (mobile phase: cyclohexane-ethyl acetate 5:1 to 1:1). This gave 670 mg (63% of theory) of the product.

1. washwashed with saturated aqueous ammonium chloride solution (3×40 ml)
2. dry with materialwith saturated aqueous sodium bicarbonate solution (40 ml), and the organic phase was dried over magnesium sulfate
3. additiondiluted
4. concentrationconcentrated
5. customThe residue was chromatographed on silica gel (mobile phase: cyclohexane-ethyl acetate 5:1 to 1:1)