Formaldehyde → HCID 86744898, compound

Participants

Reaction Steps

To 100 ml. of a 1N solution of monosodium dihydrogen phosphate are added 3.4 g. (0.02 mole) 4-(2-nitroxyethyl)-piperidine in 10 ml. dioxan. While cooling and stirring, there are now added dropwise at +10° C., 10 ml. of a 37% solution of formaldehyde in the course of 10 minutes. After stirring overnight at ambient temperature, the reaction mixture is rendered alkaline with potassium carbonate and extracted with ethyl acetate. The organic phase is dried with anhydrous sodium sulphate and distilled in a vacuum. The remaining oil is dissolved in ethanol and converted into the salt by the addition of 1.2 g. fumaric acid. After filtering off with suction, there are obtained 2 g. of the fumarate of the title compound, i.e. 33% of theory; m.p. 105°-107° C.

Provenance & Evidence