JPH05238711

PURPOSE:To improve reproducibility and safety by providing an automatic heating means, an automatic gas and liq. charging and discharging means and a means for adjusting the internal pressure of a reaction vessel to the vessel to automate hydrazinolysis. CONSTITUTION:The hydrazine anhydride stored in a reagent bottle group 18b is uniformly distributed to plural reaction vessels 12 connected to a main body 14 through a reagent adding line 18 and a liq. distributor 32 and vacuum-dried, and the hydrazine anhydride is heated to 100 deg.C by a heat block 16 and subjected to a reaction for a specified time. Heating is stopped after the reaction is finished, the vessel 12 is cooled and evacuated to remove unreacted hydrazine. The vessel 12 is returned to ordinary pressure, toluene in the reagent bottle group 18b is introduced, and the vessel is again evacuated to remove the hydrazine by the azeotropy with toluene. Aq. sodium bicarbonate is then added to quench the reaction system, and the acetic anhydride is added to substitute the hydrazide at the end of the amino acid for a hydroxyl group. The reaction product is sent to an ion-exchange column 24, stored in an eluate collecting messflask 38 and then refined.