Calcium Carbonate → benzyl N-(2-hydroxy-4-nitrophenyl)carbamate

Participants

Reaction Steps

3.58 moles (536 ml) of benzyl chloroformate (95%) are added in the course of 45 minutes to 3.25 moles (500 g) of 2-amino-5-nitrophenol and 204.5 g of calcium carbonate in 1.5 liter of dioxane brought to 70° C., the temperature being maintained at between 70° C. and 80° C. When the addition is complete, heating is maintained for a further 30 minutes. The inorganic salts present in the reaction medium are removed by filtration while hot. After the addition of ice-cold water to the filtrate, the expected product crystallizes. After filtration and drying, the product obtained is recrystallized from acetic acid. It melts at 200° C.

Provenance & Evidence