Methyl cyanoacetate → HCID 178437791, compound

Participants

Reaction Conditions

Reaction Steps

1,1-Dimethoxy-N,N-dimethylmethanamine (24.4 g) was added to a solution of methyl 3-oxopentanoate (25.4 g) in methanol (50 mL) at room temperature. The mixture was stirred at 50° C. under nitrogen atmosphere for 3 hours. After cooling to room temperature, methyl cyanoacetate (21.3 g) and N-ethyl-N-isopropylpropan-2-amine (25.2 g) were added to the reaction mixture. The mixture was stirred at 50° C. under nitrogen atmosphere for 16 hours. After cooling to room temperature, acetic acid (14.1 g) was added to the reaction mixture at 50° C. The mixture was stirred at 50° C. under nitrogen atmosphere for 10 minutes. Water (150 mL) was added to the reaction mixture at 50° C. The mixture was stirred at room temperature for 2 hours. After filtration, the crystals were washed with methanol-water (1:4) and then diisopropyl ether. The crystals were dried at 70° C. under vacuum to give the title compound (22.3 g).

Provenance & Evidence