Perdeuterated Pyridinium Ionic Liquids for Direct Biomass Dissolution and Characterization

A review of whole cell wall NMR by the direct-dissolution of biomass

“…30,31 Addressing the former issue with the use of ILs as NMR solvents, Ragauskas et al synthesized perdeuterated pyridinium chloride (PyCl-d 6 ) in a one-step procedure from commercially available deuterated pyridine in 95% yield (see Scheme 1) and established that a (1 : 2) organic electrolyte solvent of anhydrous PyCl-d 6 /DMSO-d 6 is well suited for the dissolution and NMR analysis for both Wiley-milled and ballmilled biomass. [27][28][29] Beyond PyCl-d 6 , Cheng et al…”

“…Jiang et al initially reported a PyCl-d 6 : DMSO-d 6 solvent as an effective system for the NMR characterization of biomass. [27][28][29] A (1 : 2) mixture of PyCl-d 6 : DMSO-d 6 was capable of dissolving up to 80 mg of Wiley-milled (∼80-20 mesh) and ball-milled poplar and switchgrass samples by stirring at 60 °C for 6 h in 1 mL of solvent. 1 H and 13 C NMR spectra of both the Wiley milled and ball-milled samples provided comparable spectra, generating all relevant and representative signals from both lignin and polysacchar- ides, subsequently demonstrating the exceptional solubility of biomass in the solvent system.…”