Reaktion #1536701

Reaktionsgleichung

dimethylaminopyridine

3-methyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carbonylchloride hydrochloride

3-aminopyridine

→

titled compound

3-Methyl-N-(2-pyridyl)-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carboxamide dihydrochloride

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated and to the mixture
2. 2
   workup.ADDITIONwas added saturated sodium hydrogencarbonate aqueous solution
3. 3
   ExtraktionThe mixture was extracted with chloroform
4. 4
   WaschenThe extact was washed with water
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   SonstigeThe solvent was removed under reduced pressure
7. 7
   workup.DISSOLUTIONThe residue was dissolved in ethanol
8. 8
   workup.ADDITIONTo the solution was added saturated hydrogenchloride diethylether solution
9. 9
   FiltrationThe formed crystals were collected by filtration
10. 10
    SonstigeThis crystals were recrystallized from a mixed solvent of ethanol and diethylether

Vorschrift

In 20 ml of pyridine was dissolved 200 mg of 3-aminopyridine. To this solution were added 50 mg of dimethylaminopyridine and 600 mg of 3-methyl-6,7-dihydro-5H-thiazolo[3,2-a]pyrimidine-2-carbonylchloride hydrochloride obtained in Example 28, followed by stirring at room temperature for 20 hours. The reaction mixture was concentrated and to the mixture was added saturated sodium hydrogencarbonate aqueous solution. The mixture was extracted with chloroform. The extact was washed with water and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure. The residue was dissolved in ethanol. To the solution was added saturated hydrogenchloride diethylether solution. The formed crystals were collected by filtration. This crystals were recrystallized from a mixed solvent of ethanol and diethylether to obtain 300 mg of the titled compound.

Quelle