Method for synthesizing bromoethyl acetate
A technology of ethyl bromoacetate and a synthetic method, applied in the synthesis field of ethyl bromoacetate, can solve problems such as patent documents that have not yet been found, and achieve the effects of easy control, reasonable and feasible process, and low cost
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Embodiment 1
[0023] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.
[0024] (1) Bromination: Add 70 g of acetic acid and 20 g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70° C., start to add 168 g of bromine dropwise, and finish adding in 24 hours. Add 3-5 liters of water, heat to reflux for 2 hours, filter after cooling, then distill off hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize bromoacetic acid, about 140g.
[0025] (2) Esterification: add bromoacetic acid, 72g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel remained substantially constant (19ml), the reaction was complete.
[0026] (3) Neutralization and washing with ...
Embodiment 2
[0029] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.
[0030] (1) Bromination: Add 72g of acetic acid and 20g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70°C, start to add 170g of bromine dropwise, and finish adding in 22 hours. Add 3-5 liters of water and heat to reflux for 2 hours, filter after cooling, then distill off the hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize into bromoacetic acid, about 139g.
[0031] (2) Esterification: add bromoacetic acid, 78g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel was substantially constant (18.5ml), the reaction was complete.
[0032] (3) Neutralization and washing w...
Embodiment 3
[0035] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.
[0036] Steps:
[0037] (1) Bromination: Add 75g of acetic acid and 20g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70°C, start adding 162g of bromine dropwise, and finish adding in 22.5 hours. Add 3-5 liters of water and heat to reflux for 2 hours, filter after cooling, then distill off hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize into bromoacetic acid, about 140g.
[0038] (2) Esterification: add the bromoacetic acid, 80g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel was substantially constant (17.5ml), the reaction was complete.
[0039] (3) Neutraliz...
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