تفاعل #524944

معادلة التفاعل

N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride

4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine

diethylamine hydrochloride

potassium carbonate

→

N,N-Diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine

المذيبات

ethanol

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONA mixture containing 8.2 g
2. 2
   تركيزconcentrated in vacuo to dryness
3. 3
   أخرىthe solid collected
4. 4
   workup.DISSOLUTIONThe solid was dissolved
5. 5
   workup.ADDITIONthe hot solution treated with decolorizing charcoal
6. 6
   ترشيحfiltered
7. 7
   درجة الحرارةto cool
8. 8
   workup.ADDITIONsaturated with gaseous hydrogen chloride, ether was added to turbidity
9. 9
   أخرىThe separated solid was collected
10. 10
    أخرىdried in vacuo at 80° C.
11. 11
    أخرىto yield 7.4 g

الإجراء التجريبي

A mixture containing 8.2 g. of 4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine, 8.7 g. of diethylamine hydrochloride, 100 ml. of ethanol, 6 g. of potassium carbonate and 10 ml. of water was refluxed with stirring for eight hours and then concentrated in vacuo to dryness. The residue was swirled in water and the solid collected. The solid was dissolved in boiling isopropyl alcohol, the hot solution treated with decolorizing charcoal and filtered, and the hot filtrate allowed to cool. The filtrate was then saturated with gaseous hydrogen chloride, ether was added to turbidity and the mixture was allowed to stand. The separated solid was collected and dried in vacuo at 80° C. to yield 7.4 g. of N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride, m.p. 205°-208° C.

المصدر