Electric Literature of 4331-29-7, These common heterocyclic compound, 4331-29-7, name is 1H-Benzo[d]imidazol-7-amine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Adenine (17.4 g, 0.13 mol),Sodium carbonate (15.9 g, 0.15 mol)1R-propylene carbonate (15.8 g, 0.15 mol)Was dissolved in 50 mL of N-methylpyrrolidone,Heated to 90 ~ 125 ° C,Insulation at 90 ~ 125 ° CReaction 3 ~ 6 hours;Down to room temperature,Under a argon atmosphere, magnesium tert-butoxide (23.8 g, 0.14 mol) was added,Heating up to 30 ~ 45,Insulation reaction 0.5 ~ 1 hour;DripP-toluenesulfonyloxymethylphosphonic acidDiethyl ester (48.3 g, 0.15 mol)Insulation at 30 ~ 45 ° C continue to react 4 ~ 6 hours; the system down to room temperature,The reaction system was concentrated under reduced pressure to give a viscous oily substance intermediate 2;To the resulting intermediate 2 was added 130 g of concentrated sulfuric acid,Heating up to 90 ~ 110 ° C,Insulation reaction 3 ~ 6 hours;Down to room temperature,The reaction was continued at room temperature for 1 to 2 hours,Filter,The filter cake was washed twice with 150 mL of 5 wtpercent dilute sulfuric acid aqueous solution, The filtrate with sodium hydroxide solution rhoEta = 2 ~ 3,Crystallization overnight, cooling to 0 ~ 3 ° C,So that the crystallization for 3 hours;Filter,The filter cake was washed once with 30 mL of water,50 mL of water and acetone (V / V = 1: 1) was washed twice,50mL acetone washed once;Vacuum drying,Tylenolide 31g,The total molar yield was 83.8percentHPLC purity of 98.5percent
Statistics shows that 1H-Benzo[d]imidazol-7-amine is playing an increasingly important role. we look forward to future research findings about 4331-29-7.