반응 #60861

반응 방정식

6-(1-cyclopropyl-4-phenyl-1H-imidazol-5-yl)-4-(methylthio)thieno[2,3-d]pyrimidine

Intermediate 71

6-(1-cyclopropyl-4-phenyl-1H-imidazol-5-yl)-4-(methylthio)thieno[2,3-d]pyrimidine

NH3

NH4Cl

→

title compound

수율 35.0%

6-(1-Cyclopropyl-4-phenyl-1H-imidazol-5-yl)thieno[2,3-d]pyrimidin-4-amine

수율 35.0%

용매

DCM

water

dioxane

반응 조건

후처리

1. 1
   추출The aqueous layer was extracted with DCM
2. 2
   농축the combined organics were concentrated
3. 3
   기타The crude product was purified by flash chromatography on silica eluting with Hex

실험 절차

6-(1-cyclopropyl-4-phenyl-1H-imidazol-5-yl)-4-(methylthio)thieno[2,3-d]pyrimidine (Intermediate 71) (25 mg), NH3 (aq. conc) and NH4Cl (sat. aq.) in dioxane (2 mL) were heated under microwave conditions (CEM explorer, 170° C., 4 hours). The reaction mixture was diluted with DCM and water. The aqueous layer was extracted with DCM and then the combined organics were concentrated. The crude product was purified by flash chromatography on silica eluting with Hex:EtOAc (1:1 to 100% EtOAc, then MeOH:EtOAc 95:5) to afford the title compound as a solid (8 mg, 35%);

출처