تفاعل #697989

معادلة التفاعل

4-amino-N-(2,6-bis-methylamino-pyrimidin-4-yl)-benzenesulfonamide

diazomethane

→

4-amino-N-(2,6-bis-methylamino-pyrimidin-4-yl)-N-methyl-benzenesulfonamide

المردود 35.0%

المذيبات

methanol

dimethylformamide

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONThe solvent was distilled off
2. 2
   أخرىthe residue was chromatographed over 50 g of SiO2 with 5% of methanol in methylene chloride as the eluent

الإجراء التجريبي

0.65 g (0.0021 mol) of 4-amino-N-(2,6-bis-methylamino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in a mixture of 100 ml of methanol and 400 ml of dimethylformamide and treated with 60 ml of a solution of diazomethane in diethyl ether. The mixture was stirred at room temperature for 30 minutes. The solvent was distilled off and the residue was chromatographed over 50 g of SiO2 with 5% of methanol in methylene chloride as the eluent. There was obtained 0.24 g (35%) of 4-amino-N-(2,6-bis-methylamino-pyrimidin-4-yl)-N-methyl-benzenesulfonamide as a yellow solid; m.p.: 79-80° C.

المصدر