反应详情

To a solution of methyl 6-(4-fluorophenyl)-2-methoxy-4-methyl-1,6-dihydro-5-pyrimidinecarboxylate (1.76 g, 6.34 mmol) and 4-dimethylaminopyridine (12.7 mmol, 1.55 g) in anhydrous CH2Cl2 (20.0 mL) was added solution of 4-nitrophenyl chloroformate (4.47 g, 22.2 mmol) in CH2Cl2 (20.0 mL) at 23° C. The reaction mixture was stirred for 2 hours at room temperature. The reaction mixture was diluted with CH2Cl2 (50 mL), washed with water, brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash column chromatography (hexanesiethyl acetate 4:1). The product was obtained as yellow syrup, which upon trituration with hexanes became a white powder (2.40 g, 84.3%). The crude product was used in next step without further purification.

1. washwashed with water, brine
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe residue was purified by flash column chromatography (hexanesiethyl acetate 4:1)
5. customThe product was obtained as yellow syrup, which upon trituration with hexanes
6. customThe crude product was used in next step without further purification