تفاعل #465454

معادلة التفاعل

4-amino-N-(6-chloro-2-ethylamino-pyrimidin-4-yl)-benzenesulfonamide

trimethylamine

methylamine hydrochloride

→

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

المردود 54.0%

المذيبات

ethanol

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONtreated in an ultrasound bath for 15 minutes
2. 2
   ترشيحThe precipitate was filtered off
3. 3
   workup.DISSOLUTIONdissolved in 150 ml of 1N NaOH
4. 4
   ترشيحfiltered
5. 5
   ترشيحThe precipitate was filtered off under suction
6. 6
   غسيلwashed with water
7. 7
   أخرىdried

الإجراء التجريبي

0.1 g (0.00031 mol) of 4-amino-N-(6-chloro-2-ethylamino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in 20 ml of ethanol and stirred with 0.6 ml (0.0043 mol) of trimethylamine and 0.1 g (0.0015 mol) of methylamine hydrochloride in an autoclave at 130° C. for 4 hours. The reaction mixture was freed from solvent, the residue was suspended in 5 ml of ethanol and treated in an ultrasound bath for 15 minutes. The precipitate was filtered off, dissolved in 150 ml of 1N NaOH and filtered. The filtrate was adjusted to pH 6 with 0.1N HCl. The precipitate was filtered off under suction, washed with water and dried. There was obtained 0.053 g (54%) of 4-amino-N-(2-ethylamino-6-methylamino-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p.: 261-263° C.

المصدر