The invention provides a one-pot preparation method of ethyl 4-bromobutyrate, which is characterized by comprising the following steps: step 1, adding gamma-butyrolactone into an
organic solvent, and carrying out
reflux water separation while dropwise adding a
hydrobromic acid aqueous solution, step 2, detecting the content of gamma-butyrolactone, if the content is less than 0.5% by
mass fraction, carrying out step 3, and if the content is more than 0.5% by
mass fraction, carrying out step 4; 3, dropwise adding absolute ethyl
alcohol, continuing to carry out
reflux water separation until the
water content is less than 0.2% by
mass fraction to obtain a crude product solution of the ethyl 4-bromobutyrate, and carrying out
distillation and rectification to obtain a purified ethyl 4-bromobutyrate solution, and 4, detecting the water in the
system, and if the
water content is less than 0.5% by
mass fraction, carrying out the step 3, and if the
water content is less than 0.5% by
mass fraction, carrying out the step 4. If not, continuously supplementing and dripping the
hydrobromic acid aqueous solution, continuously carrying out
reflux water diversion, and repeating the step 2; when the water content is 0.5% or above by
mass fraction, continuing to carry out reflux water separation, and repeating the step 2.