반응 #157266

반응 방정식

water

(2-chloro-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl)-(3-morpholin-4-ylmethyl-phenyl)-amine

1-(4-chloro-phenyl)-piperazine

diisopropylethylamine

→

product

수율 74.5%

{2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl}-(3-morpholin-4-ylmethyl-phenyl)-amine

수율 74.5%

용매

dioxane

반응 조건

후처리

1. 1
   추출the mixture is extracted with dichloromethane
2. 2
   기타The organic phase is separated off
3. 3
   기타evaporated to dryness
4. 4
   기타The residue is crystallised with methanol

실험 절차

1.09 g (2-chloro-6,7-dihydro-thieno[3,2-d]pyrimidin-4-yl)-(3-morpholin-4-ylmethyl-phenyl)-amine, 1.77 g 1-(4-chloro-phenyl)-piperazine and 1.03 ml diisopropylethylamine are placed in 12 ml dioxane, then heated in the microwave for 1 hour at 160° C. Then water is added and the mixture is extracted with dichloromethane. The organic phase is separated off using a phase transfer cartridge and evaporated to dryness. The residue is crystallised with methanol. 1.17 g of the product are obtained as a powder (m.p 177°-178° C.).

출처