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dimethyl-2-(2-butylimidazol-1-yl)succinate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
39%
With 1,8-diazabicyclo[5.4.0]undec-7-ene; In acetonitrile; at 25℃; for 3h;
In a 100 ml flask with an inlet of four, 9.5 g (0.06 mol) of diazabicyclo undecene (DBU) , 18 ml of acetonitrile, 17.1 g (0.14 mol) of <strong>[50790-93-7]2-butylimidazole</strong> was added and the mixture was stirred at 25 C. In addition, 18.0 g (0.12 mol) of dimethyl fumarate was added dropwise and reacted at 25 DEG C for 3 hours. After completion of the reaction, the Extraction was carried out with 70 ml of methylene chloride and 50 ml of water, after removing the solvent under reduced pressure. The collected organic layer was concentrated by separation, and the obtained concentrate was purified by silica gel column chromatography (ethyl acetate / hexane = 1/1) , to obtain 2- (2-butyl-imidazol-1-yl) dimethyl succinate as a liquid phase. The obtained 2- (2-butyl-imidazol-1-yl) dimethyl succinate, yield 13.1g was 39%.2- (2-butylimidazol-1-yl) succinic acid dimethyl, and a release reaction of the protective group start under a temperature condition of 179 , and the disappearance of dimethyl succinate in 2- (2-butyl-imidazol-1-yl) dimethyl succinate was confirmed by NMR analysis. In addition, in GC analysis, it was confirmed that dimethyl fumarate originating from the leaving protecting group A was produced.
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