Kod studija u vezi sa sintezom kloramfenikola (ikloromicetina) prireden je dosada neopisani dietilni ester dikloracetamidomalonske kiseline

V. Tomašić

Croatian

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AR HIV Z A K E M I J U 24 (1952) Priprava dietilnog estera dikloracetamidomalonske kiseline V . TOMASIC 103 Kod studija u vezisa sintezom kloramfenikola (ikloromicetina) prireden j e dosada neopisani dietilni ester dik1oracetamidoma..lonske Mseline.* K otopini od 2,l g (0,01 mol) Mdrnklorida amfoomalonskog estera') i. 1,43 g ro,01 mol) dii:ldio1racetilklori.d1a?) u 30 ccm suhog benzena1, poste-peno se do<l.a 1,58 g (0,02 mola) piridina u 10 cam suhog henzena uz mje-Sa.nje i hladenje ledom. Smjesa se ostavi stajati pireko noci kod sobne tern· perature. Benz.enski se 1sloj otfiltrira, opere V'Odom i ,SiUJSi sa Na2SO,. Iza -uklanjanja suvifoog otapafa .desti:lacijom, produkt se ipn~kri·staHzfra iz hen· zena. Dobive:no je 1,7 •g· (61°/o) bijelih i;glica, T. t. 104-105°. Za anaHzu suiblimirano kod 119-121° (0.02 mm) Hg 12,410 m:g tvari .daje 17,25 ~ C02 i 5,16 mg H20. C9H1 30 5NC12 1(i2861.03) Rae~ C: 37,760/o H: 4,58°/ci Nad. IC: 37,930/ij H: 4,650/o I·STRAz'lV AoKI ODJ.EL :»PLIVA« TVORN~CA LIJEKOVA ZAGREB ABSTRACT P:dmljeno 25. sijecnja 1952. Preparation of Diethyl Ester of Dichloracetamidomalonic Acid V. TOMASIC A new diethyl ester of dfohlomcetamid-0m1a1lonic E11Ci.d hais been p 1re,pared. To a solutio n containini? 2.l J!. (0.01 imol) Olf the hydroichloride o.f aminoma11onic -es'ter am<l/ 1.43 ~- (0.01 mol) of dfohinroacetyilchlo11i1de d!n 30 c. c. of .dry benzene 1.58 g. '(0.02 mOil} of pyridine i!ll 10 c. c. o f dry benzene is· aidded s'l!Jcccsisdvely ·under ·constant '5tiilr.rdng and coo,~mg wii:th ice. Tihe mdxture, a:fte.r hei'!lJg neft staindilng ovemilght at "l"O()ffi terrlll?eMture, iJS fJ.Itered and 'the .benzene soiuiti·Q!Il, washed w.iith w~ter a.nd dnied wii1fih so1drium s'1.lllipihrute. The exc.e;ss· lheneene dis removed lby d i;sti,llai!Ji10in. and the 01b!Jadned diethyl ester of dichloracetamidomalonic acid CuH130sNCb, recrystam1zed ·from benzene. Ycidd 61 O/o, m. IP· 10~105°. RESEAROH DEPARTMENT »PLIVA« :!PHARMACEUTICAL AND CHEMICAL PRODUCTS ZAGREB , CROATIA: [Received , January 25, 1952] * ZaihvaJj:ujem se Upiravii tvorniice ,!~jeko;v.a »PM'Va« na, dozvioJJil z.a olbj1avilj1rva.nje <OVog Te~Ul~taita,, ,kao .i Dir. L. Filiipo1v1i6u, na Kem. inst. prir. mat. faikuHeta u Za1gre1bu .za izvil:isene miJkroan.a1ize. · .1> A. G :a11l a. it, J. Am. Ohem. Soc., 69 (1947) 965 ; Z. Ve j de I ek, C., 1951 1324; p .Jiio ty i Neresche~mer, Ber., 39 (1906) 514; 56 (1923) 22'14; Snyder :i Sm ·i t h, J. Am. Oh em. Soc., 66 (1944) 350. 2) He rh er t C. B r O· w n, J. Am. Ohern. Soc., 60 (1938) 1325. 

Priprava dietilnog estera dikloracetamidomalonske kiseline

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