GB595431A - Improvements in or relating to the isolation of piperazine - Google Patents

Improvements in or relating to the isolation of piperazine

Info

Publication number
GB595431A
GB595431A GB9319/45A GB931945A GB595431A GB 595431 A GB595431 A GB 595431A GB 9319/45 A GB9319/45 A GB 9319/45A GB 931945 A GB931945 A GB 931945A GB 595431 A GB595431 A GB 595431A
Authority
GB
United Kingdom
Prior art keywords
piperazine
solution
hydrohalide
double salt
ammonium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB9319/45A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhone Poulenc SA
Original Assignee
Rhone Poulenc SA
Societe des Usines Chimiques Rhone Poulenc SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rhone Poulenc SA, Societe des Usines Chimiques Rhone Poulenc SA filed Critical Rhone Poulenc SA
Publication of GB595431A publication Critical patent/GB595431A/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
    • C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
    • C07D295/023—Preparation; Separation; Stabilisation; Use of additives

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

Piperazine is isolated in the form of its hydrohalide/ammonium halide double salt from an aqueous solution containing a piperazine hydrohalide by adding to the heated solution a quantity of an ammonium halide in excess of the stoichiometric amount (relative to the piperazine hydrohalide), cooling and separating from the solution the resulting precipitate of the piperazine hydrohalide-ammonium halide double salt. The solution so treated is advantageously one containing a piperazine hydrohalide mixed with hydrohalides of other organic bases with or without mineral salts, or one obtained by the conversion of diphenyl piperazine into the nitroso compound, followed by treatment with bisulphite and hydrolysed in an acid medium, or by the method disclosed in Specification 595,430. In examples: (1) a mixture containing 181 parts piperazine hydrochloride (obtained by the method of Specification 595,430) is dissolved in 1000 parts water and the warmed solution is treated with 200 parts ammonium chloride and thereafter cooled to precipitate the double salt; (2) a solution of piperazine (obtained from diphenyl piperazine via its nitroso compound) is concentrated, freed from precipitated salts, treated with concentrated ammonia to bring the pH to 2 and then with ammonium chloride to precipitate the double salt. A sample has been furnished under Sect. 2 (5) of the double salt of piperazine hydrobromide and ammonium bromide, obtained by p neutralizing an aqueous solution of piperazine hydrate with aqueous hydrobromic acid and by adding to the warmed solution ammonium bromide, followed by cooling.
GB9319/45A 1944-04-21 1945-04-13 Improvements in or relating to the isolation of piperazine Expired GB595431A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR595431X 1944-04-21

Publications (1)

Publication Number Publication Date
GB595431A true GB595431A (en) 1947-12-04

Family

ID=8966854

Family Applications (1)

Application Number Title Priority Date Filing Date
GB9319/45A Expired GB595431A (en) 1944-04-21 1945-04-13 Improvements in or relating to the isolation of piperazine

Country Status (1)

Country Link
GB (1) GB595431A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1067820B (en) * 1955-07-28 1959-10-29 Boots Pure Drug Co Ltd Process for the production of piperazine
US3023211A (en) * 1960-09-12 1962-02-27 Jefferson Chem Co Inc Method for the preparation of piperazine monohydrochloride

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1067820B (en) * 1955-07-28 1959-10-29 Boots Pure Drug Co Ltd Process for the production of piperazine
US3023211A (en) * 1960-09-12 1962-02-27 Jefferson Chem Co Inc Method for the preparation of piperazine monohydrochloride

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