1-(5-Chloro-2-methylphenyl)piperazine synthesis

Yield: 83.9%

Reaction Conditions:

with potassium iodide in chlorobenzene for 24 h;Reflux;

Steps:

1.4 (4) Synthesis of 1-(5-chloro-2-methylphenyl)piperazine:
Weighed 4.2.48 g (0.3 mol) of 5-chloro-2-methylaniline,57.11 g (0.32 mol) of bis(2-chloroethyl)amine hydrochloride and 5.0 g of KI (0.03 mol),300 ml of chlorobenzene was added as a solvent and refluxed for 24.0 h. After sufficient cooling, suction filtration,The mother liquor is evaporated to dryness to recover the solvent to give a reddish brown oil.Add a small amount of acetone to dissolve under heating.After cooling, the solid precipitated, suction filtered and combined with the previous solid.Add 150ml of acetone and reflux for 1.0h-2.0h. After cooling, filter to obtain white powder solid.(62.2g, 83.9%),When the dosage is increased to 1.2 mol, the yield is increased to 89.0%.

References:

The Chinese People's Liberation Army Military Academy Of Medical Sciences Poison Pharmaceutical Institute;Li Jin;Yang Rifang;Song Rui;Wu Ning;Li Yunfeng;Wang Weina;Song Dake CN109419802, 2019, A Location in patent:Paragraph 0114; 0120