Methyl 2-(2-Methyl-3-Thiosemicarbazido)-2-Oxoacetate置于amberlite Ir 120 (H) Resin,1,8-二氮杂双环[5.4.0]十一碳-7-烯体系中,化学反应生成 2,5-二氢-6-羟基-2-甲基-5-氧-3-巯基-1,2,4-三嗪 参考文献:Synthesis Of 6-Hydroxy-2-Methyl-3-Thioxo-2H-1,2,4-Triazin-5-One 标题:Synthesis Of 6-Hydroxy-2-Methyl-3-Thioxo-2H-1,2,4-Triazin-5-One 摘要:The Title Compound Has Been Prepared In Three Steps From 2-Methylthiosemicarbazide Following Acylation,Cyclisation And Cation Exchange Chromatography. It Was Fully Characterised By The Usual Spectroscopic Means As Well As By N-15 NMR Spectroscopy And X-Ray Crystallographic Analysis. DOI:10.1080/00397919608003566
专利信息
专利号:US-5945414-A 优先权日:1996-12-03 标 题:Process for the preparation of new intermediates useful in the synthesis of cephalosporins 发明人:SOGLI LORIS; TERRASSAN DANIELE; BERNASCONI ERMANNO; SALTO FRANCISCO 权利人:ANTIBIOTICOS SPA 摘要:Cefazolin, cefazedone, cefoperazone, cefamandole, cefatrizine or ceftriaxone is prepared by reacting glutaryl 7-ACA of the formula: with a compound of formula (II): R-SH(II) wherein R is 5-methyl-1,3,4-thiadiazol-2-yl, 1H-1,2,3-triazol-4-yl, 1-methyl-tetrazol-5-yl or 1,2,5,6-tetrahydro-2-methyl-5,6-dioxo-1,2,4-triazin-3-yl group, and R1 and R2 are both hydrogen and the other is an acyl group, in an aqueous solution in an amount of 3-5 mols per mol of glutaryl 7-ACA to about 90 DEG C. and for a time from about 2 to about 10 hours; optionally recovering the excess of the compound of formula (II), thereby preparing a compound of formula (III) in an aqueous solution: wherein R is as above defined and optionally deacylating said compound of formula (III); and converting the resulting compound of formula (I) wherein R, R1 and R2 are as defined above in the presence of a non-chlorinated solvent into one of said cephalosporins.
专利号:US-5387679-A 优先权日:1991-07-15 标题 :Process for the preparation of cephalosporins intermediates 发明人:SOGLI LORIS; TERRASSAN DANIELE; RIBALDONE GIUSEPPE 权利人:ANTIBIOTICOS SPA 摘要:PCT No. PCT/EP92/01595 Sec. 371 Date Mar. 15, 1993 Sec. 102(e) Date Mar. 15, 1993 PCT Filed Jul. 14, 1992 PCT Pub. No. WO93/02085 PCT Pub. Date Feb. 4, 1993.The present invention relates to a process for preparing a compound of formula (I) ntains at least one nitrogen atom with or without oxygen or sulphur and R1 and R2 are both hydrogen atoms or one of them is an hydrogen atom and the other is an acyl group; the process comprising reacting a compound of formula (II) (II) wherein R1 and R2 are each as defined above, and wherein, if necessary, any reactive group is protected by a suitable protective group, or a salt thereof, with a compound of formula (III) R-SH(III) wherein R is as defined above, or a salt thereof, in the presence of an acid and of a compound of formula (IV) (IV) wherein each of R3 and R4 is a C1-C4 alkyl group or R3 and R4 taken together are a C2 or C3 alkylene chain and, if necessary, removing the protective groups possibly present. The compounds of formula (I) are useful intermediates in the synthesis of Cefazolin and Cefazedone.
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专利号:EP-0846695-A1 优先权日:1996-12-03 标题:Process for the preparation of new intermediates useful in the synthesis of cephalosporins
专利号:IT-MI962533-A1 优先权日:1996-12-03 标 题 :PROCEDURE FOR THE PREPARATION OF INTERMEDIATES USEFUL IN THE SYNTHESIS OF CEPHALOSPORIN
专利号:KR-19980063587-A 优先权日:1996-12-03 标 题:Method for preparing novel intermediates useful for the synthesis of cephalosporins