反应详情

A solution of crude 1-[(dimethylamino)carbonyl]-1,6-dihydro-2-methoxy-4-methyl-6-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methylethyl ester (2.27 g), in tetrahydrofuran/methanol (20 ml each) was treated with 5N hydrochloric acid (3.0 ml, pH1) and stirred at room temperature for 1.0 hour. The reaction was then evaporated and partitioned between ethyl acetate and water. The organic phase was washed with saturated sodium chloride, dried (magnesium sulfate), and evaporated. The residue was crystallized from dichloromethane/isopropyl ether to give the title compound as colorless crystals (1.55 g), melting point 165°-166° C.

1. customThe reaction was then evaporated
2. custompartitioned between ethyl acetate and water
3. washThe organic phase was washed with saturated sodium chloride
4. dry with materialdried (magnesium sulfate)
5. customevaporated
6. customThe residue was crystallized from dichloromethane/isopropyl ether