3,5-DICHLORO-2-HYDROXYBENZALDEHYDE HYDRAZONE synthesis

Yield:43002-22-8 96%

Reaction Conditions:

with hydrazine hydrate in methanol; for 3 h;Reflux;

Steps:

3.3 Typical procedure for preparation of hydrazinomethylphenols. Preparation Method III (see Scheme 4)

General procedure: Preparation of 2-(hydrazonomethyl)-4-nitrophenol (SA33). A mixture of methanol (300ml), 2-hydroxy-5-nitrobenzaldehyde (250mg; 1.5mmol), and hydrazine monohydrate (130mg; 4.5mmol) was refluxed for three hours. The solvent was evaporated to a solid residue. This residue was mixed with hot methanol (10ml) and sonicated at 60°C for a few minutes. The resulting mixture was mixed with water (～100ml) and then cooled in ice bath. The resulting insoluble product was separated by filtration, washed with cold water (3×5ml) and dried under reduced pressure to give pure product (230mg; 85%).

References:

Backes, Gregory L.;Neumann, Donna M.;Jursic, Branko S. [Bioorganic and Medicinal Chemistry,2014,vol. 22,# 17,p. 4629 - 4636]