Sulfuric Acid → 4-O-Hexopyranosyl-N-[hydroxy(imino)methyl]hexopyranosylamine

Participants

Reaction Steps

360 g of lactose monohydrate (1 mole) were mixed with 60 g of urea (1 mole) and 10.6 ml of a solution made up of 100 ml of H2O and 6 ml of 98% H2SO4. The mixture was melted and deposited as a thin layer on the moving belt of a tunnel oven. This oven was equipped with a system for controlling its temperature in a first third of its length (zone I) according to a temperature gradient and, in the second 2/3 of its length (zone II), at a constant temperature. Zone I was subjected to a temperature gradient ranging from ambient, at the entrance, to 100°-110° at the end of zone I; zone II was maintained at a constant temperature of 100°-110° C. The mixture coated on the belt thus penetrated into the tunnel and was gradually heated, in 11/2 hrs, to 110° after which it entered zone II where it stayed for 2-3 hrs at 110° C. At the exit of the tunnel, the mixture was cooled and had the aspect of a slightly foamy, crystalline, light brown material, easy to remove from the belt with a doctor-knife and which could be ground into a powder. This product was collected in a continuous manner and about 400 g were obtained.

Provenance & Evidence