Synthesis method for 2,3-dibromo-1,4-butylene glycol
A technology of butene diol and synthesis method, which is applied in the separation/purification of hydroxyl compounds, organic chemistry, and the preparation of halogens, which can solve the problems of reduced yield, product process loss, low temperature and difficult suction filtration, etc., and achieve reduction The loss of solvent, beneficial to recycling, the effect of simple and easy method
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Embodiment 1
[0028] A method for synthesizing 2,3-dibromo-1,4-butenediol, comprising the following steps:
[0029] 1) Preparation of brominating agent tetraethylammonium bromide complex bromide:
[0030] In a four-necked flask equipped with an electric stirrer and a thermometer, add 150ml of dichloromethane, add 110g of tetraethylammonium bromide, add 82.4g of liquid bromine dropwise while stirring, and react for 1 hour until the reaction is complete. Brominating agent tetraethylammonium bromide complex bromide;
[0031] 2) Preparation of crude 2,3-dibromo-1,4-butenediol:
[0032] In the dichloromethane solvent, add butynediol and the brominating agent tetraethylammonium bromide complex bromide prepared in step 1) to undergo electrophilic addition reaction to generate 2,3-dibromo-1,4 -butenediol; wash with water, lower the temperature to crystallize 2,3-dibromo-1,4-butenediol, and filter to obtain 2,3-dibromo-1,4-butenediol Crude product: the mol ratio of the butynediol added in the ste...
Embodiment 2
[0036] 3) Purification of crude 2,3-dibromo-1,4-butenediol:
[0037] In a four-neck flask equipped with a condenser tube, an electric stirrer, and a thermometer, add the crude 2,3-dibromo-1,4-butenediol obtained in step 2) and 250 g of water, start stirring, and raise the temperature to control the temperature Stir at 80-90°C to dissolve the material completely, add 6g of sodium sulfite to remove residual bromine, add 5g of activated carbon for decolorization treatment: the decolorization process is 80-90°C and heat preservation reaction for 1.5 hours, heat suction filtration, and cool the filtrate to 0-5 °C, recrystallize the purified 2,3-dibromo-1,4-butenediol, filter it with suction, and dry the filter cake under vacuum at room temperature to obtain pure white 2,3-dibromo-1,4- Butenediol; bromine content 64.97%, yield 80%, purity 99.4%.
Embodiment 3
[0039] Mother liquor all reclaims and applies mechanically the method for synthesizing 2,3-dibromo-1,4-butenediol, comprises the following steps:
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