反应详情

温度

0 °C

A suspension of 2-amino-4-methyl-6-(3-nitrophenyl)-1,5(6H)-pyrimidinedicarboxylic acid, diethyl ester (600 mg, 1.59 mmoles, see Example 2) in dichloromethane (5 ml) and pyridine (1.0 ml) was cooled to 0° C. under argon and was treated dropwise with methanesulfonyl chloride (0.42 ml, 5.26 mmoles). A catalytic amount of 4-dimethylamionpyridine was added and the reaction was allowed to warm to room temperature. After stirring overnight, the reaction was diluted with ethyl acetate and was washed with 1N hydrochloric acid, sodium bicarbonate and brine. It was dried over anhydrous magnesium sulfate and the solvent was evaporated to provide a colorless residue. Crystallization from ether-hexanes provided the title compound as a colorless crystalline material, melting point 139°-140.5° C.

1. additionA catalytic amount of 4-dimethylamionpyridine was added
2. temperatureto warm to room temperature
3. washwas washed with 1N hydrochloric acid, sodium bicarbonate and brine
4. dry with materialIt was dried over anhydrous magnesium sulfate
5. customthe solvent was evaporated
6. customto provide a colorless residue
7. customCrystallization from ether-hexanes