反应详情

Triethylamine (0.88 g, 8.70 mmol) was added to a solution of ethyl 4-(2-(4-(2-hydroxyethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (1.50 g, 4.37 mmol) in methylene chloride (40 ml). The mixture was stirred under ice-cooling, and methanesulfonyl chloride (0.60 g, 5.24 mmol) was added dropwise to the mixture. The resulting mixture was stirred under ice-cooling for 10 minutes after the addition. Then, water (40 ml) was added to the reaction mixture. The mixture was extracted with methylene chloride and dried over magnesium sulfate. After evaporation of the solvent, the residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (=1/1) to give the desired ethyl 4-(2-(4-(2-methylsulfonyloxyethyl)phenyl)ethylamino)-6-ethylpyrimidine-5-carboxylate (1.80 g, 98%).

1. temperaturecooling
2. stirringThe resulting mixture was stirred under ice-
3. temperaturecooling for 10 minutes
4. additionafter the addition
5. extractionThe mixture was extracted with methylene chloride
6. dry with materialdried over magnesium sulfate
7. customAfter evaporation of the solvent
8. customthe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (=1/1)