Piperazin-1-yl-acetic acid methyl ester hydrochloride synthesis

Yield:196192-08-2 64%

Reaction Conditions:

Stage #1: piperazine dihydrochloride in methanol;Heating;
Stage #2: methyl chloroacetatewith copper(II) ions supported on commercial polymeric resin at 20;Microwave irradiation;Flow reactor;

Steps:

Microwave flow reactor experiments (C)

started in the same manner and thus at first a solutionof piperazine monohydrochloride or piperazine monoacetate was prepared in the same way andpoured into a reservoir flask of a flow reactor. Subsequently, a catalyst (0.5: 1 mol. with respect to acorresponding reagent) was loaded into a reaction flask placed in a MW oven (a detailed scheme isdescribed on Scheme 2). Then pump was switched on to run the flow slowly (approx. 2-5 mL.s1).A corresponding reagent was added portion wise (possibility of a turbulent reaction) into the reservoirflask to be introduced into the reaction mixture. The microwave oven power was always set to aminimal energy (10% of a maximal power, i.e., 80 W) and then applied using a pulse mode (typically 3sec. of a set power then pause for 4 sec.) to keep the mixture in the reaction flask only slightly boiling.

References:

?ev?ík, Richard;?imbera, Jan;Havránková, Eva;Něme?ková, Dana;Pazdera, Pavel [Molecules,2020,vol. 25,# 9]