Process for the preparation of N-(2-sulfatoethyl)-piperazine in

Details Process for the preparation of N-(2-sulfatoethyl)-piperazine in Process for the preparation of N-(2-sulfatoethyl)-piperazine in

1995-03-15

1997-01-21

Bernhardt, Emily

Organic compounds -- part of the class 532-570 series

Organic compounds

Nitrogen attached directly or indirectly to the purine ring...

C07D295088

Patent

active

055960995

ABSTRACT:
A process for the preparation of N-(2-sulfatoethyl)-piperazine in high purity, which comprises reacting N-(2-hydroxyethyl)piperazine in a mixture of highly--or relatively highly--concentrated sulfuric acid and oleum or chlorosulfonic acid at temperatures of from about 80.degree. to about 250.degree. C., transferring the resulting sulfonation mixture to a water-miscible aliphatic alcohol, isolating the N-(2-sulfatoethyl)piperazine sulfate formed, treating the N-(2-sulfatoethyl)piperazine sulfate, still moist with alcohol, at temperatures of from about 35.degree. to about 90.degree. C. with a basic compound in a mixture of a (C.sub.1 -C.sub.2)-alkanol and water, separating off the precipitated sulfate of the basic compound employed, and isolating the N-(2-sulfatoethyl)piperazine formed, by the addition of (C.sub.1 -C.sub.2)-alkanol.

REFERENCES:
patent: 3194822 (1965-07-01), Goldstein
Organic Functional Group Preparations by Stanley R. Sandler and Wolf Karo, vol. III p. 116-124 (1972).
Research Techniques in Organic Chemistry by Robert B. Bates, John P. Schaefer, pp. 50,51,55 (1971).
Tomalia et al, J. Het. Chem. 9, pp. 891-894 (1972).
Andrew Streitweiser, Jr., "Introduction to Organic Chemistry", Second Edition, p. 815 (1981).
Barton & Ollis, "Comprehensive Organic Chemistry", vol. 3, p. 370 (1979).

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