Sulfuric Acid → HCID 86736818, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 72 g of 1-(5-aminocarbonyl-pentyl)-3-(2-cyanoacetyl)-urea, 125 ml of water, 125 ml of dioxane, 23.2 g of sodium nitrite and 1 ml of acetic acid was adjusted to pH 4.5 to 5 at 50° C. by slowly adding 15% strength sulphuric acid dropwise. The reaction mixture was stirred at 50° C. for 2 hours, diluted with 600 ml of water and 600 ml of ethyl acetate, then cooled at 20° C. and adjusted to a pH value of 2. The crystals were separated off, washed with water and dried in vacuo. 61.3 g of 1-(5-aminocarbonyl-pentyl)-3-(2-cyano-2-oximinoacetyl)-urea of melting point 187°-189° C. were obtained.

Provenance & Evidence