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ChemicalBook CAS DataBase List 2-(DiMethoxyMethyl)-5-(MethoxyMethyl)furan
110339-34-9

2-(DiMethoxyMethyl)-5-(MethoxyMethyl)furan synthesis

8synthesis methods
-

Yield:-

Reaction Conditions:

with silica-supported nickel phosphide at 150; under 750.075 Torr; for 3 h;Inert atmosphere;Autoclave;

Steps:



General procedure: For catalytic experiments, a stainless-steel batch reactor of 100mL (Parr Instrument) was charged with a catalyst (100mg), furanyl substrate, and solvent (19mL) in which the substrate concentration was set at 0.21M. The reactor was then purged with inert N2 at 25°C for 1h and heated to a desired temperature (usually, 150°C). The reaction started with stirring at 600rpm and was performed for 3h. After the reaction was complete, the heating and stirring were stopped and cooled to 25°C. From the collected etherification product mixture, a sample (1.5mL) was taken and then mixed with 0.08g of toluene (99.5 %) that is an external standard for GC analysis using an Agilent 7890A GC with a flame ionization detector (FID) and a INNOWAX capillary column (30m × 0.25mm × 0.25μm). While the injector and detector were set at 250 and 300°C, respectively, the oven temperature was programmed as follows: 40°C for 2min, ramping to 160°C at 20°Cmin-1, holding at 160°C for 2min, followed by ramping to 250°C at 10°Cmin-1, and finally holding at 250°C for 5min. The product was confirmed by GC-MS analysis (Agilent INNOWAX column). For quantitative measurement, the experiments were repeated at least three times and the average product compositions were reported in this context. Finally, the conversion of furanyl alcohol and the selectivity and yield of each product were calculated as follows:

References:

Kim, Jinsung;Shin, Mi;Suh, Young-Woong [Applied Catalysis A: General,2020,vol. 603]