Guanidine → HCID 178513087, compound

Participants

Reaction Steps

To a solution of 0.072 mols guanidine (from 6.9 g guanidine hydrochloride and 3 g NaOH) in 100 ml water, 20 g (0.06 mols) 2-(2,6-dichlorophenyl)-2-bromo-acetyl-bromide in 50 ml acetone and 2.4 g (0.06 mols) NaOH in 50 ml water at 10 degrees C. are simultaneously added dropwise. After one hour, the organic phase is extracted with methylene chloride, filtered, and further extracted in a counter-current manner with 1 N hydrochloric acid. The acid phase is then adjusted to an alkaline pH and extracted with CH2Cl2. Subsequent to the evaporation of the methylene chloride, the guanidine base is obtained. It has decomposition point of 155 degrees C. The hydrochloride is prepared in the usual way using ethanolic hydrochloric acid, and is recrystalized from a mixture of acetic acid and ethanol. The decomposition point is 228-229 degrees C.

Provenance & Evidence