تفاعل #2468010

معادلة التفاعل

2-chloro-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-dimethylamino-pyrimidine

water

hydrochloric acid

4-dimethylaminomethyl-phenylamine

→

2-(4-dimethylaminomethyl-phenylamino)-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-dimethylamino-pyrimidine

المذيبات

DMF

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   أخرىThe suspension obtained
2. 2
   أخرىpurified by column chromatography
3. 3
   أخرىThe fractions are freeze-dried
4. 4
   أخرىfreeze-dried once more

الإجراء التجريبي

50 mg 2-chloro-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-dimethylamino-pyrimidine are suspended in 60 μL of 1,4-dioxane, 20 μL water and 90 μL of a 5 M hydrochloric acid (in 1,4-dioxane) and mixed with 55 mg 4-dimethylaminomethyl-phenylamine. This mixture is heated to 95° C. and stirred for 20 h at this temperature. The suspension obtained is diluted with DMF and then purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which consists at the starting point of 95% water (10 mM ammonium hydrogen carbonate and 38 mM ammonia) and 5% acetonitrile and at the finishing point of 50% water and 50% acetonitrile. The fractions are freeze-dried. The residue is taken up in acetonitrile, combined with aqueous hydrochloric acid and freeze-dried once more.

المصدر