ES262759A1 - A method for the preparation of n, n, n-triethylenethiophosphoramide - Google Patents

A method for the preparation of n, n, n-triethylenethiophosphoramide

Info

Publication number
ES262759A1
ES262759A1 ES0262759A ES262759A ES262759A1 ES 262759 A1 ES262759 A1 ES 262759A1 ES 0262759 A ES0262759 A ES 0262759A ES 262759 A ES262759 A ES 262759A ES 262759 A1 ES262759 A1 ES 262759A1
Authority
ES
Spain
Prior art keywords
diethyl ether
metallo
derivative
ethyleneimine
stirring
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
ES0262759A
Other languages
Spanish (es)
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.)
SIMES Societa Italiana Medicinali e Sintetici SpA
Original Assignee
SIMES Societa Italiana Medicinali e Sintetici SpA
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 SIMES Societa Italiana Medicinali e Sintetici SpA filed Critical SIMES Societa Italiana Medicinali e Sintetici SpA
Publication of ES262759A1 publication Critical patent/ES262759A1/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02—Phosphorus compounds
    • C07F9/06—Phosphorus compounds without P—C bonds
    • C07F9/22—Amides of acids of phosphorus
    • C07F9/224—Phosphorus triamides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
    • C07F9/02—Phosphorus compounds
    • C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
    • C07F9/553—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having one nitrogen atom as the only ring hetero atom
    • C07F9/564—Three-membered rings

Abstract

N,N1,N11-triethylenethiophosphoramide is obtained by reacting an N-metallo derivative of ethyleneimine with a phosphorus thiohalide at between -30 DEG C. and +15 DEG C. in an inert anhydrous organic solvent. The N-metallo derivative may be obtained by transmetallation between a metallo-alkyl and ethyleneimine and is preferably an alkali metal or alkaline earth metal derivative and the molar ratio of phosphorus thiohalide to the N-metallo derivative is suitably between 1 : 3 and 1 : 3.5. Specified organic solvents are ethers, e.g. diethyl ether, diisopropyl ether, or the dimethylether of diethylene glycol. In an example methyllithium dissolved in anhydrous diethyl ether is added with stirring to ethyleneimine dissolved in anhydrous diethyl ether and the precipitate formed is held in suspension by stirring in the same solvent suspension is then poured slowly into a cooled solution of PSBr3 in anhydrous diethyl ether. The temperature is not allowed to rise above +5 DEG C. and after further stirring at room temperature the mixture is filtered and the ether p evaporated to dryness to yield a residue comprising N,N1,N11-triethylene-thio-phosphoramide. Specification 729,586 is referred to.
ES0262759A 1959-11-26 1960-11-25 A method for the preparation of n, n, n-triethylenethiophosphoramide Expired ES262759A1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB4026159A GB894820A (en) 1959-11-26 1959-11-26 A method for the preparation of n, n, n-triethylenethiophosphoramide

Publications (1)

Publication Number Publication Date
ES262759A1 true ES262759A1 (en) 1961-01-01

Family

ID=10414014

Family Applications (1)

Application Number Title Priority Date Filing Date
ES0262759A Expired ES262759A1 (en) 1959-11-26 1960-11-25 A method for the preparation of n, n, n-triethylenethiophosphoramide

Country Status (2)

Country Link
ES (1) ES262759A1 (en)
GB (1) GB894820A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3227728A (en) * 1963-11-26 1966-01-04 Monsanto Res Corp Preparation of diimidazol-1-yl derivatives of phosphine oxide
CN109956972A (en) * 2017-12-22 2019-07-02 四川科瑞德凯华制药有限公司 Phosphinothioylidynetrisaziridine crystal form I and its preparation method and application

Also Published As

Publication number Publication date
GB894820A (en) 1962-04-26

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