Isolation of Methyl Esters from Fatty Acids Over Mesoporous V/SBA-15

Electronic Supplementary Information

Isolation of Methyl esters from Fatty acids over Mesoporous V/SBA-15

V. Udayakumara, A. Pandurangana,b,*

a Department of Chemistry, Anna University, Guindy, Chennai 600 025, India

b Institute of Catalysis and Petroleum Technology, Anna University, Chennai 600 025, India

Fig. S1 1H NMR spectra (500 MHz, CDCl3) of sunflower oil.

It reveals the presence of four methylene hydrogen (-CH2-O-) in the region of 4.1 and 4.3 ppm, methine hydrogen (–CH-) in the region of 5.2 ppm and olefinic hydrogen (–CH=CH-) in the region of 5.3 ppm. From the expansion 1H NMR of sunflower oil two quartet signals of -CH2- protons were observed clearly in the region of 4.15 and 4.3 ppm due to the splitting of adjacent –CH- proton and also a quintet signal of –CH- was observed in the region of 5.2 ppm due to the splitting of adjacent two –CH2- protons.

* Corresponding author at: Department of Chemistry, Anna University, Guindy, Chennai-600 025, India. Tel.: +91 44 22358653; fax: +91 44 22200660.

E-mail address: (A.Pandurangan).

Fig. S2 1H NMR spectra (500 MHz, CDCl3) of fatty acid methyl ester.

In this we can see the absence of –CH2-O- protons and –CH- proton signals of glycerol, instead of that methoxy (CH3-O-) proton was observed clearly as a singlet in the region of 3.7 ppm.

Fig. S3 1H NMR spectra (500 MHz, DMSO-d6) of glycerol.

Glycerol is the byproduct in the transesterification of sunflower oil and methanol, it is soluble in polar solvents like water and methanol, the aqueous phase of the reaction mixtures contains glycerol and traces of ester. The aqueous phase was rotaevaporated at 80 °C after the complete removal of water, Thin layer chromatography (TLC) was checked using 40% methanol and 60% chloroform as an eluent to identify the product (Rf = 0.4) and it was purified by column chromatography using 60-120 mesh silica. Nonpolar impurities were isolated in plain chloroform, at 2% methanol and chloroform glycerol was isolated and the structure was identified using 1H NMR spectroscopy, singlet signal was observed in the region of 4.5 ppm it reveals the presence of three hydroxyl (–OH) protons, two methylene (–CH2-) protons in the region of 3.6 ppm and one methine (–CH-) proton in the region of 3.1 ppm were observed.

Fig. S4 1H NMR spectra (500 MHz, DMSO-d6) of methyl butyrate.

Fig. S5 1H NMR spectra (500 MHz, DMSO-d6) of methyl pentanoate.

Fig. S6 1H NMR spectra (500 MHz, DMSO-d6) of methyl octanoate.

Fig. S7 1H NMR spectra (500 MHz, DMSO-d6) of methyl oleate.