Process for the preparation of N-(2,3-Dihydrobenzo[1,4]dioxin-2-carbonyl)piperazine
AssigneeCouncil of Scientific and Industrial Research
InventorsMalladi Pardhasaradhi, Gullapalli Kumaraswamy, Arun Kanti Das, Nivedita Jena, Chembumkulam Kamalakshyamma Snehalatha Nair, Mudiganti Naga Venkata Sastry
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Abstract
Described herein is an improved process for the preparation of N-(2,3-Dihydrobenzo[1,4]dioxin-2-carbonyl)piperazine which includes heating a reaction mixture ethyl of 2,3-dihydrobenzo[1,4]dioxin-2-carboxylate and piperazine. The reaction mixture is then subjected to series of washes and extraction to yield N-(2,3-Dihydrobenzo[1,4]dioxin-2-carbonyl)piperazine having a purity of greater than 99.9%.
Claims4
A process for the preparation of N-(2,3-Dihydrobenzo[1,4]dioxin-2-carbonyl)piperazine which comprises heating a reaction mixture ethyl of 2,3-dihydrobenzo[1,4]dioxin-2-carboxylate and piperazine with a molar ratio of carboxylate to piperazine in the range of 1:2 to 2:1, under nitrogen atmosphere, at a temperature in the range of 70-90° C. for a period of 3-15 hrs, cooling the above said reaction mixture to a temperature of 25-30° C. and dissolving it in chloroform followed by washing with saturated sodium bi-carbonate solution and water respectively, acidifying the organic layer by about 10% HCl to a pH ranging between 1 to 4, separating the organic layer and washing the aqueous layer with chloroform, basifying the aqueous layer with sodium bi-carbonate to a pH ranging between 7 to 9 followed by extracting with chloroform and evaporating the chloroform to obtain the final desired product in amorphous solid form.
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