Acetate → 4-Nitrophenol

Beteiligte Stoffe

Reaktionsschritte

A solution of 10 mg of calcitonine M acetate in 2 ml of absolute dimethylformamide is treated with 0.5 ml of a 1% solution of para-nitrophenylacetate in dimethylformamide, rinsed with nitrogen, and allowed to stand in the closed test tube at 40°C for 30 minutes. 5 ml of 2N-acetic acid are then added, the excess para-nitrophenyl acetate and the para-nitrophenol formed are extracted with ethyl acetate (2 × 30 ml), the aqueous phase is evaporated to dryness under reduced pressure, the residue dissolved in 0.5 ml of 95% acetic acid, and the solution lyophilized. The product consists of a mixture of mono- and diacetyl derivative and some starting material. The monoacetyl derivative itself is a mixture of the Nα- and Nε-derivatives as evidenced by electrophoresis at pH 8.

Herkunft & Nachweise