[Na].Cl[C:3]1[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=1.[CH2:13]([OH:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>>[CH2:13]([O:20][C:3]1[N:4]=[N:5][C:6]([S:9][CH2:10][CH:11]=[CH2:12])=[CH:7][CH:8]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=10.11 g(0.005 mol) of metallic sodium was dissolved in 20 ml of dry benzylalcohol. To the resulting solution was added 0.93 g(0.005 mol) of 3-chloro-6-allylthiopyridazine and then the reaction solution was stirred for 2 hours at 80±5° C. To remove the excessive benzylalcohol and the insoluble material (NaCl), the reaction mixture was purified with silica gel column chromatography (eluent: n-hexane/ethyl acetate=40/1, v/v) to obtain the title compound as a needle crystal.
Wird geladen…