تفاعل #465469

معادلة التفاعل

4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide

methylamine hydrochloride

triethylamine

→

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

المردود 45.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىthe residue was partitioned in ethyl acetate/water
2. 2
   ترشيحthe insoluble constituents were filtered off under suction
3. 3
   أخرىThe filter cake was recrystallized in methanol/diethyl ether

الإجراء التجريبي

0.62 g (0.0019 mol) of 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in 10 ml of ethanol, treated with 1.67 g (0.025 mol) of methylamine hydrochloride and 6.2 ml (0.044 mol) of triethylamine and stirred in an autoclave at 140° C. for 18 hours. The mixture was freed completely from solvent, the residue was partitioned in ethyl acetate/water and the insoluble constituents were filtered off under suction. The filter cake was recrystallized in methanol/diethyl ether. There was obtained 0.28 g (45%) of N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-chloro-benzenesulfonamide as white crystals; m.p. 272-273° C.

المصدر