2,2-dimethylene dioxy group 1,3-propylene glycol carbonate, preparation method and application thereof
A technology of dimethylene dioxyl and propylene glycol carbonate, which is applied in the direction of organic chemistry, can solve the problems of complex operation, long time required, and low yield, and achieve simple operation, short reaction time, and high yield Effect
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example 1
[0021] At room temperature, slowly add (preferably within 2 hours) 50.0 g (0.23 mol) of 1 to 300 ml of anhydrous tetrahydrofuran suspension containing 11.88 g (0.31 mol) of lithium aluminum hydride in an argon atmosphere, 200 ml of tetrahydrofuran solution of 3-dioxolane-2,2-dicarboxylate, then reacted for 2 hours, added 50 ml of ethyl acetate to decompose excess lithium aluminum hydride, then added 50 ml of water, The reaction was continued for 2 hours. Filter, wash the solid 3 times with 100 ml tetrahydrofuran, combine the filtrates and dry with anhydrous sodium sulfate, evaporate the solvent under reduced pressure, and distill the residual liquid under reduced pressure, collect the fraction at 130-2°C / 35Pa to obtain 22.54 g of colorless or light yellow Viscous liquid 1,3-dioxolane-2,2-dimethanol, yield 73%.
example 2
[0023] At 0°C, add 13.40 g (0.1 mol) of 1,3-dioxolane-2,2-dimethanol and 22.80 g (0.21 mol) of ethyl chloroformate in 500 ml of anhydrous THF A mixture of 22.6 g (0.1 mol) of triethylamine in 50 ml of anhydrous tetrahydrofuran was slowly added (over 1.5 hours) and the reaction was continued at room temperature for 2 hours. After the reaction was completed, it was filtered, and the filtrate was concentrated to obtain a residue, which was then recrystallized from ethyl acetate to obtain white needle-like crystals of 2,2-dimethylenedioxy-1,3-propanediol carbonate with a yield of 47%. The melting point is 96-97° C. FTIR (KBr): 1751.9 (vs, C=O), 1183.8, 1095.7, 1131.3 cm -1 (vs, C-O-C). 1 H NMR (CDCl 3 ): δ=4.239 (4H, s, CH 2 OCOCH 2 ), 4.049 (4H, s, OCH 2 CH 2 O). 13 C NMR (CDCl 3 ): δ=147.136 (C=O), 99.474 (quarter C), 70.730 (CH 2 OCOCH 2 ), 64.898 (OCH 2 CH 2 o).
example 3
[0025] Slowly add (1.5 hours Inner added) containing 50 ml of anhydrous dichloromethane mixed solution of 11.88 g (0.04 mol) triphosgene, then back distillation 2.5 hours. After the reaction, it was concentrated to 100 ml, washed 3 times with 50 ml of water, dried over magnesium sulfate, filtered, evaporated to remove the solvent, and the residue was recrystallized from ethyl acetate to obtain white needle-like crystals of 2,2-dimethylene dioxygen Base-1,3-propanediol carbonate, yield 40%.
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