反应详情

A solution of 1,6-dihydro-2-methoxy-4-methyl-6-(3-nitrophenyl)-1-[[(phenylmethyl)amino]carbonyl]-5-pyrimidinecarboxylic acid, 1-methylethyl ester (3.00 g, 6.45 mmol) in tetrahydrofuran (50 ml)/methanol (25 ml) was treated with 1 N hydrochloric acid (6.0 ml, pH 1) and stirred at room temperature for 1 hour. The reaction was quenched with saturated sodium bicarbonate and partially evaporated. The residue was partitioned between chloroform and water. The organic phase was washed with saturated sodium chloride, dried (magnesium sulfate) and evaporated. The residue was crystallized from dichloromethane/isopropyl ether. The solids which precipitated were recrystallized to give the title compound as a colorless electrostatic solid (1.84 g), melting point 184°-185° C. TLC (5% ethyl acetate/dichloromethane) single spot, Rf =0.39.

1. customThe reaction was quenched with saturated sodium bicarbonate
2. custompartially evaporated
3. customThe residue was partitioned between chloroform and water
4. washThe organic phase was washed with saturated sodium chloride
5. dry with materialdried (magnesium sulfate)
6. customevaporated
7. customThe residue was crystallized from dichloromethane/isopropyl ether
8. customThe solids which precipitated
9. customwere recrystallized