The desiccant in the mixture was able to remove most of the water so as to provide a suitable anhydrous condition under which the reaction proceeded to completion, and the desired crude hydrazone 1 was obtained in a pleasing 90% yield (Scheme 2). The crude was then purified using flash column chromatography (80% EtOAc in cyclohexane; R f 0.25) to obtain 1 in high purity ~ p.a. ≥98%, as evidenced by H NMR (Fig. ), LC-MS and HRMS (ESI S2 †), and intriguingly in marked contrast to that of the literature as an orange solid (Fig. ) in 62% yield. Ultra-pure samples of 6 and 7 were also obtained using the newly devised method (ESI S5 & S6 †), alongside 2 (ESI S3 †) for comparison with 1. Hydrazone 1 is quite insoluble in most common organic solvents such as ether, dichloromethane, toluene, chloroform etc., but sparingly soluble in acetonitrile and fairly soluble in DMSO. To this end, a relatively clean 1 H NMR spectrum of 1 in acetonitrile-d 3 was first obtained; however, the exchangeable protons, in the absence of deuterons, complicate the overall trace integration of the thus obtained spectrum: this was rectified by means of a 'D 2 O shake', nevertheless, hardly surprisingly, even traces of residual water from the added D 2 O reacted with 1 so as to give rise to minor inexplicable new peaks at  8.55, 7.53, 7.52, 7.27 and 7.26 (Fig. ). It cannot be too firmly emphasised that unlike clean 1 H NMR spectra of 1 in acetonitrile-d 3 , the 1 H NMR spectrum of 1 in methanol-d 4 was a complete mess (Fig. ), this clearly shed light on reactivity of methanol towards 1; thus any attempt at synthesis of this compound in methanolic solutions could lead to highly impure products. Knowing that methanol reacts with 1, it was then investigated as to whether methanol in lieu of the nucleophile i.e. hydrazine would also react with the starting material, namely, 5-nitrofurfural, in such syntheses. Unlike 1, 5-nitrofurfural is sufficiently soluble in chloroform; to this end, its 1 H NMR spectrum in CDCl 3 was obtained and compared with that in methanol-d 4 . It did not come as a surprise to discover that similar but different to 1, 5-nitrofurfural is equally susceptible to attack by methanol as its 1 H NMR spectrum in methanold 4 contains extra signals in the region  7.5 -5.5, which were absent in its obtained spectrum in CDCl 3 (Fig. ).