The invention provides a synthetic method of guanethidine subplate
drug intermediate
cycloheptanone. The synthetic method comprises the following steps: (1) adding 500 to 600ml of water, 1.5mol of
metal powder, a
phosphoric acid solution with the
mass fraction of 40 to 50 percent into a reaction vessel provided with a stirrer, a
thermometer and a
dropping funnel, wherein the solution temperature is controlled to be 60 to 70 DEG C, dropwise adding 1.2mol of nitromethylcycloheanol, after adding, maintaining the solution temperature at 40 to 50 DEG C, adding 30mL of
sulfuric acid solution with the
mass fraction of 40 to 45 percent for 3 times every 30min, and maintaining the solution pH at 3 to 4 for 1h, wherein filter liquor is aminomethlcycloheanol
sulfate liquor, and a filter liquor cake is used for the next batch after being washed by using a
solvent; (2) regulating the solution pH to 2 to 3 by using
sulfuric acid, reducing the solution temperature to 2 to 5 DEG C, slowly adding and dissolving 1.5 to 2mol of
sodium sulfite in 200ml of water, then heating up to 30 to 35 DEG C, distilling by using steam till a non-oily matter is distilled off, separating out an oil layer, extracting a
water layer for 10 to 15 times by a
solvent, combining the oil layer and a
solvent layer, distilling off the solvent at normal pressure, then performing reduced pressure
distillation, and collecting 65 to 70 DEG C
cut fraction to obtain the
cycloheptanone.