Hydrochloric Acid → HCID 22749250, compound

Participants

Reaction Conditions

Reaction Steps

11 g of N-carbethoxy acetyl N-methyl o-nitro aniline are admixed with 16.2 g of powdered zinc, and 100 g of cracked ice are added, whilst agitating; 62 c.c. of concentrated hydrochloric acid, diluted with 250 c.c. of iced water, are then added, and this is cooled to -5°-10° C for 10 to 15 minutes; the temperature is allowed to raise again to + 5° C within thirty minutes, this is filtered, the filtrate is alkalinized with ammonium hydroxide and extracted with chloroform; the chloroformic phases are washed with water, dried over sodium sulfate and evaporated under reduced pressure; the residue is dissolved in 30 c.c. of xylene and the solution is kept overnight at -10° C; the formed precipitate is washed with ether and recrystallized in xylene, to obtain N-carbethoxy acetyl N-methyl o-phenylene diamine, melting at 63°-64° C. Analysis: C12H16N2O3 = 256.26; Calculated: C % 61.00; H % 6.83; N % 11.86; Found: 61.19; 6.98; 12.00.

Provenance & Evidence