DE926488C - Process for the preparation of neutral esters of thiophosphoric acid - Google Patents

Process for the preparation of neutral esters of thiophosphoric acid

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Publication number
DE926488C
DE926488C DEF12003A DEF0012003A DE926488C DE 926488 C DE926488 C DE 926488C DE F12003 A DEF12003 A DE F12003A DE F0012003 A DEF0012003 A DE F0012003A DE 926488 C DE926488 C DE 926488C
Authority
DE
Germany
Prior art keywords
preparation
thiophosphoric acid
neutral esters
esters
neutral
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
DEF12003A
Other languages
German (de)
Inventor
Walter Dr Lorenz
Gerhard Dr Schrader
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.)
Bayer AG
Original Assignee
Bayer AG
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 Bayer AG filed Critical Bayer AG
Priority to DEF12003A priority Critical patent/DE926488C/en
Application granted granted Critical
Publication of DE926488C publication Critical patent/DE926488C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/16Esters of thiophosphoric acids or thiophosphorous acids
    • C07F9/165Esters of thiophosphoric acids
    • C07F9/17Esters of thiophosphoric acids with hydroxyalkyl compounds without further substituents on alkyl

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)

Description

Verfahren zur Herstellung von neutralen Estern der Thiophosphorsäure In der Patentschrift 818 352 Ist ein Verfahren zur Herstellung von neutralen Estern der Thiophosphorsäure beschrieben, das darin besteht, daß man auf die Al!kaliisalze von Dialkylphosphiten Alkylrbodandde einwirken läßt.Process for the preparation of neutral esters of thiophosphoric acid In patent specification 818 352 is a process for the preparation of neutral esters the thiophosphoric acid described, which consists in the fact that one on the alkali metal salts from dialkyl phosphites alkylrbodandde to act.

Es wurde nun gefunden, daß neutrale Ester der Thiophosphorsäure leicht zugängh-Ch sind, wenn man, Alkylrlhodanide mit Triralkylphbsph,iten umsetzt. Die Umsetzung erfolgt bei erhöhter Temperatur, gegebenenfalls in einem indifferenten Lösungs@mnttel. Auf diese Weise wird bei der Herstellung der gewünschten Thiopihosphors,äu-reester das Arbeiten mit Alkalimetallen, insbesondere metallischem Natrium, vermieden. Der Umsetzung liegt folgendes Reaktionsschema zugrunde Beispiel 1 17 g Triäthylphosphit werden in 3o ccm Xylol gelöst. Unter Rühren gibt man bei 11d° 14,7 9 ß-Äthy lmercapto-äthylrr!hodanid ;hinzu und entfernt gleichzeitig das Wärmebad. Die Temperatur steigt von selbst auf 14o°'. Man riihrt bei dieser Tempe- ratur noch 1.5 Minuten weiter,, und fraktioniert dann das Rohprodukt. Es werden" i3 g des o, o-Diäthyl- S-,B-äthylmeTcapto-äthylthiophosphats vom Kp2 132 bis 13q:° erhalten. Ausbeute 52%. Beispiel. 2 26g .Athylrhodanid werden in 5o ccm Triäbhyl- phosphit -kn Kölbehen mit freier Flamme biss, zum Eintritt der Reaktion erwärmt. Die Temperatur steigt ratsch,ara-f 130 bis 135'°. Nach Erkalten erhält man durch Fraktionierung 21 g o, o, S-Triäthyl- thiophospha:t. Ausbeute 36%. It has now been found that neutral esters of thiophosphoric acid are easily accessible if, alkyl rhodanides are reacted with tri-alkyl phosphates. The reaction takes place at elevated temperature, if appropriate in an inert solution. In this way, working with alkali metals, in particular metallic sodium, is avoided in the production of the desired thiophosphorus, outer esters. The implementation is based on the following reaction scheme Example 1 17 g of triethyl phosphite are dissolved in 3o cc of xylene. While stirring, at 11d ° 14.7 9 β-ethyl mercapto-ethyl-rhodanide is added and the heating bath is removed at the same time. The temperature rises by itself to 14o ° '. One stirs at this temperature rature another 1.5 minutes, and then fractionates the raw product. "I3 g of the o, o-diethyl S-, B-ethylmeTcapto-ethylthiophosphate of bp2 132 to 13q: ° obtained. Yield 52%. Example. 2 26g .Athylrhodanid are in 5o ccm Triäbhyl- phosphite -kn Kölbehen with a free flame bit, to Heated entry of the reaction. The temperature rises ratsch, ara-f 130 to 135 °. Receives after cooling one by fractionation 21 go, o, S-triethyl- thiophospha: t. Yield 36%.

Claims (1)

PAT-ENTANSPRUCH: Weitere Ausbildung,des Verfahrens zur Her- stellung von neutralen Estern der 'fhsophosphor- säure nackt Patent 818 352, dadurch gek-enn- zeithnet, daB Alky1rhodanide hier mit T:rialkyl- phosphiten bei erhöhter Temperatur zur Um- . setzung gebracht werden.
PAT CLAIM: Further training, the procedure for production of neutral esters of the 'phsophosphorus acid naked patent 818 352, thus recognized It is timed that alky1rhodanides here with T: rialkyl- phosphites at elevated temperature to . settlement are brought.
DEF12003A 1953-05-31 1953-05-31 Process for the preparation of neutral esters of thiophosphoric acid Expired DE926488C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEF12003A DE926488C (en) 1953-05-31 1953-05-31 Process for the preparation of neutral esters of thiophosphoric acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEF12003A DE926488C (en) 1953-05-31 1953-05-31 Process for the preparation of neutral esters of thiophosphoric acid

Publications (1)

Publication Number Publication Date
DE926488C true DE926488C (en) 1955-04-18

Family

ID=7086893

Family Applications (1)

Application Number Title Priority Date Filing Date
DEF12003A Expired DE926488C (en) 1953-05-31 1953-05-31 Process for the preparation of neutral esters of thiophosphoric acid

Country Status (1)

Country Link
DE (1) DE926488C (en)

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