3-Chloro-1,2-propanediol → HCID 20446520, compound

Participants

Reaction Conditions

Reaction Steps

0.2 mol (33.4 g) of 2-methyl-4-amino-5-nitroaniline and 0.1 mol (10 g) of calcium carbonate, suspended in 100 ml of water, are heated beforehand on a boiling water-bath, whilst stirring. 0.216 mol (24 g) of 1-chloropropane-2,3-diol is added. The reaction mixture is heated for 24 hours on the boiling water-bath, seven portions each containing 0.035 mol (3.5 g) of calcium carbonate and 0.066 mol (7.3 g) of 1-chloropropane-2,3-diol being added, one every three hours. The hot reaction mixture is filtered and the filtrate is diluted with 60 ml of water. After cooling for 24 hours at 0° C., the expected product, which has crystallised, is filtered off. The product is washed with water and recrystallised three times from ethanol. It melts at 150° C.

Provenance & Evidence