DEP0036735DA - Process for the preparation of a new derivative of trimethyl acetic acid - Google Patents

Process for the preparation of a new derivative of trimethyl acetic acid

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Publication number
DEP0036735DA
DEP0036735DA DEP0036735DA DE P0036735D A DEP0036735D A DE P0036735DA DE P0036735D A DEP0036735D A DE P0036735DA
Authority
DE
Germany
Prior art keywords
water
preparation
aur
recrystallization
new
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
Other languages
German (de)
Inventor
Friedrich Dr. Berlin Boedecker
Hans Dr. Berlin Volk
Original Assignee
Riedel-de Haen AG, Seelze
Publication date

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Description

Verfahren aur Herstellung eines neuen Abkomiilinns dei?Method of making a new agreement dei?

TPlvalinsäurel-x
thylcssigsliure/^aaurcn geiieinaaeichnetj daß men Pentaeryth broiahycLrin mit sauren Oxydationsmitteln^ vorsugsweiae mit Salpe*fcer— säure * oxydiert»
TPlvalinsäurel-x
Thylcssigsliure / ^ aaurcn denotes that pentaeryth broiahycLrin is oxidized with acidic oxidizing agents ^ as a precautionary measure with nitric acid *

Claims (1)

f.L i 12 J1 ί υ j fJ. I PJ fL i 12 J1 ί υ j fJ. I PJ Verfahren zur Here teilung eines neuen Abfeccmilings ^.er g e ο β i^8 äur e ( Pi valins äur e ) <■ Method for the division of a new Abfeccmilings ^ .er ge ο β i ^ 8 aur e (Pi valins aur e) <■ Sy mm· £x±bron^riinetliylessigsäure ζ^ -^1-Dibrom-ß-brorimethyl propan~J3-carbo2isäure) war bisher noeii niciit bokaiint*;Es wurde dens daß man diese Verbindung erhält, wenn man Pentaerythrit^tri— bronliydrin mi"fe sauren Osyö.ationsmitteln9 yoraugsv/eis-e mit Salpetersäure» oxydierteSy mm x £ x ± bron ^ riinetliylessigsäure ζ ^ - ^ 1 dibromo-.beta.-brorimethyl propane ~ J3 carbo2isäure) was bokaiint been noeii niciit *; It was the s to obtain this compound, if you pentaerythritol tri- ^ bronliydrin 9 yoraugsv / eis-e were oxidized with nitric acid with acidic ossifying agents Der nach vorliegendem Verfahren zugängliche neue Abkb'iamlixrg der Pivalinsäure soll als Zwischenprodukt zur Herstellung the^apsutisch verwertbarer Stoffe dienen»The new abbreviation of pivalic acid accessible according to the present process is intended as an intermediate product for the preparation of the apsutic recyclable materials serve » Beispielt 16 92 g Pentaerythrit-tribromhydrin werden in ein Gemisch au© 60 g 98^10Ö?»iger Salpetersäure und 20 g Wasser untei gutem Bühren bei 80-90° portions?/eise eingetragen* Dann wird noch so lange w eiTsr erwärmt« bis die Entwicklung von Stickoxyden praktisch aufgehört hat* Beim Erkalten erstarrt die in der Wärme gum !Teil als öl ausgeschiedene &jnwi* Sribron-pivalinsäure vollkoxnmen Icriatallin« Man verdünnt mit ca» 100 ecm Wasser» saugt ab» wäscht gut mix Wasser nach und trocknet« Ausbeute 15»5 g» lurch Umkristallisieren aus Benaol oder Gsdblin erhält man sie rein vom Fg?98~99°» (Das Säurechlorid schmilzt nach dem Umkristallisieren aus Petroläther bei 112-114°; der leth^/lester aus d es Chlorid in üblicher Weise gewonnen* hat den F/»es47-'49 *Example 16 9 2 g of pentaerythritol tribromohydrin are added in portions to a mixture of 60 g of 98% nitric acid and 20 g of water at 80-90 °. has until the evolution of nitrogen oxides virtually ceased * on cooling solidifies the gum in the heat! jnwi part as an oil secreted & * Sribron-pivalic vollkoxnmen Icriatallin "It is diluted with ca» 100 cc water "sucks" washed thoroughly mix water and dried " Yield 15.5 g. By recrystallization from Benaol or Gsdblin, they are obtained pure from 98-99 ° (the acid chloride melts after recrystallization from petroleum ether at 112-114 °; the ethyl ester from the chloride in the usual way Way won * has the F / » es 47-'49 *

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