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三嗪基苯硫甲基磺酰脲的合成 总被引:2,自引:0,他引:2
苯硫甲基磺酰胺(1)与4,6-二氯-2-三嗪异氰酸酯以碳酸钾为触媒在甲苯中加热回流制得N-4,6-二氯-2-三嗪基苯硫甲基磺酰脲(2),后者进一步与甲醇钠作用得N-4,6-二甲氧基-2-三嗪基苯硫甲基磺酰脲(3)。化合物3d经测试,具有一定的除草活性。 相似文献
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为寻找有效的抗肿瘤药物,作者对1,2,4-三嗪类化合物(6-氮杂尿嘧啶)的化学性质进行了研究,发现3-甲硫基-5-羟基-1,2,4-三嗪(1)在无水吡啶中与对甲苯磺酰氯发生不正常的对甲苯磺酰化反应,生成N-[6-(3-甲硫基-5-负氧基)-1,2,4-三嗪基]吡啶内鎓盐以及对甲苯磺酸对甲苯硫酚酯。为了研究其反应机理,把溶剂改为等摩尔NaOH的CH_3COCH_3-H_2O溶液,重复文献的实验。反应产物分离提纯后,确定其结构为3-甲硫基-4-对甲苯磺酰基-5-氧代-6-羟基-1,4,5,6-四氢-1,2,4-三嗪(2a)。此反应特点是:在1,2,4-三嗪环的4-氮上 相似文献
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自木糖经过五步反应合成了2,3-内醚-5-去羟-β-D-核糖甲基甙(Ⅵ)。这五步反应是:D-木糖(Ⅰ)→D-木糖甲基呋喃甙(Ⅱ,α-和β-端基差向异构体混合物)→2,3,5-三-O-对甲苯磺酰基-β-D-木糖甲基呋喃甙(Ⅲ)→2,3-二-O-对甲苯磺酰基-5-去羟-5-碘代-β-D-木糖甲基呋喃甙(Ⅳ)→2,3-二-O-对甲苯磺酰基-5-去羟-β-D-木糖甲基甙(Ⅴ)→2,3-内醚-5-去羟-β-D-核糖甲基甙(Ⅵ)。总产率是18%。将已知的结晶的2-O-对甲苯磺酰基-β-D-木糖甲基呋喃甙(Ⅶ)进行对甲苯磺酰化,得到与上述完全相同的Ⅲ,这样就证明了Ⅲ的端基的构型。同时,也从β-D-木糖甲基吡喃甙(Ⅷ)制备了2,3,4-三-O-对甲苯磺酰基-β-D-木糖甲基吡喃甙(Ⅸ)。根据现有的知识肯定了合成的内醚糖的结构。 相似文献
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N-对甲苯磺酰基乙二胺分别与1,11-二碘-3,6,9-三氧杂十一烷和1,14-二碘-3,6,9,12-四氧杂十四烷反应,制得N-(2-对甲苯磺酰胺基乙基)单氮杂-12-冠-4或15-冠-5;当用N-(2-对甲苯磺酰胺基乙基)二乙醇胺与1,11-二对甲苯磺酸酯-3,6,9-三氧杂十一烷反应时,才能获得N-(2-对甲苯磺酰胺基乙基)单氮杂-18-冠-6.从甲醇溶液中培养得N-(2-对甲苯磺酰胺基乙基)单氮杂-12-冠-4单晶,属单斜晶系,P21/a空间群;a=1.4229(1)nm,b=0.9595(2)nm,c=1.4564(1)nm,β=102.20(1)°,V=1.9435nm3,Z=4.最终偏离因子R=0.043. 相似文献
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六对甲苯磺酸甘露醇酯的合成 总被引:5,自引:0,他引:5
首次以甘露醇和对甲苯磺酰氯为原料,合成了六对甲苯磺酸甘露醇酯,讨论了多种因素对醇化反应收率的影响,并对其结构进行了确定。结果表明,获得六对甲苯磺酸甘露醇酯最佳的反应条件为:以100mL吡啶为溶剂兼催化剂,对甲苯磺酰氯与D-甘露醇的摩尔比为0.315:0.050,反应时间为4h。反应温度为0~10℃,收率可达85.4%。 相似文献
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磺酰氨基酸钛配合物对Diels-Alder反应的对映选择性催化作用 总被引:3,自引:0,他引:3
研究了对甲苯磺酰基-L-缬氨酸、对甲苯磺酰基-L-苯丙氨酸、对甲苯磺酰基-L-亮氨酸、对甲苯磺酰基-L-异亮氨酸、对甲苯磺酰基-L-脯氨酸、1-萘磺酰基-L-缬氨酸、1-萘磺酰基-L-苯丙氨酸、1-萘磺酰基-L-亮氨酸和1-萘磺酰基-L-异亮氨酸与钛的配合物对环戊二烯与丙烯酸甲酯的环加成反应的对映选择性催化作用。萘磺酰基氨基酸钛配合物的对映选择性比对甲苯磺酰基氨基酸钛配合物好,氨基酸与钛比为2:1时比1:1要好得多。1-萘磺酰基-L-异亮氨酸与钛的2:1配合物的对映选择性最好,e.e.值为56%。 相似文献
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Krzysztof E. Krakowiak Guoliang Yi Jerald S. Bradshaw 《Journal of heterocyclic chemistry》1996,33(6):2013-2017
1,8,15-Triazacycloheneicosane ( 1 ); 1,9,17-triazacyclotetracosane ( 2 ) and 1,10,19-triazacycloheptacosane ( 3 ) were prepared by treating the appropriate N,N-bis(ω-bromoalkyl)toluenesulfonamide 8–10 with the appropriate N,N′-ditosyl-α,ω-diaminoalkane 11–13 in dimethylformamide using sodium hydride as the base followed by phenol and 33% hydrobromic acid in acetic acid to remove the tosyl protecting groups. 2-Allyloxymethyl-4,11,18- triazaoxacycloheneicosane ( 4 ) was prepared in two ways. First, N,N′,N″-tritosylbis(hexamemylene)triamine ( 18 ) was treated with 2-allyloxymethyl-3-oxa-1,6-hexanediol ditosylate ( 23 ) and cesium carbonate in dimethylformamide followed by sodium amalgam to remove the tosyl protecting groups. The second preparation of 4 was done by treating the tri-BOC analog of 18 with 23 followed by hydrochloric acid in isopropyl alcohol to remove the BOC protecting groups. The overall yields of 4 using these two processes were very close. 相似文献
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Aminoarylhydroxy thioalkenes react with tosyl derivatives to provide mainly N substituted -2 vinyl -2,3 dihydrobenzothiazoles. A different regiochemistry of cyclization depending on whether a methyl or a phenyl susbtituent was used, was observed Formation of -2H-3,4-dihydrobenzothiazines and dienes was observed. 相似文献
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Jerald S. Bradshaw John M. Guynn Steven G. Wood Bruce E. Wilson N. Kent Dalley Reed M. Izatt 《Journal of heterocyclic chemistry》1987,24(2):415-419
Four new 14-crown-4 macrocyclic ligands containing either a pyridine or a 4-pyridone subcyclic unit have been prepared. Two of the 4-pyridono-crowns contained lipophilic hydrocarbon substituents. The starting octyl- and benzyl-substituted 4-oxa-1,7-heptanediols were prepared from the 2-octyl- or 2-benzyl-1,3-propane-diol. When the two substituted 4-oxa-1,7-heptanediols were treated with tosyl chloride, both the expected 2-substituted-4-oxaheptane-1,7-ditosylates and the ditosylate of the dimeric diol were isolated. X-ray structure determinations were carried out on two of the new 14-crown-4 compounds. 相似文献
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用KBH_4,CaCl_2为还原剂使D及L缬氨酸甲酯还原得到光学活性产物R-3-甲基-2-氨基丁醇(2a)及S-3-甲基-2-氨基丁醇(2b)。2a,2b同CS_2在KOH存在下反应得到(R)-4-异丙基四氢噻唑-2-硫酮(3a)及(S)-4-异丙基四氢噻唑-2-硫酮(3b)。肉桂酰氯分别同3a及3b在Et_3N存在下反应得到N-肉桂酰(R)-4-异丙基四氢噻唑-2-硫酮(4a)及N-肉桂酰(S)-4-异丙基四氢噻唑-2-硫酮(4b)。用半经验的量子化学PM3方法研究了反应物和产物的电子结构,得到了产物的最优构型和电荷键序分布以及反应焓变。 相似文献
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F. Bonati A. Burini B.R. Pietroni M. Felici 《Journal of organometallic chemistry》1984,273(2):275-281
Reaction of LAuCl with various pyrazol-5-ones and alkali in homogeneous or heterogeneous medium has given several 1-R-3-R′-4(LAu)2-pyrazol-5-one derivatives (R = H, phenyl, p-bromophenyl, tosyl, methyl; R′ = methyl, trifluoromethyl; L = Ph3P or Et3P). In the case of 1-aryl-5-methylpyrazol-3-one 1-aryl-2-triphenylphosphinegold-5-methylpyrazol-3-one, a compound with an AuN bond is formed. The scope, limitation, and characteristic of the auration reaction are discussed. 相似文献
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Ambident 1,2-diamines derived from the nitro-Mannich reaction containing both a tosyl amide and a secondary amine could be regioselectively cyclised through the tosyl amide onto a pendant primary hydroxyl group to give piperazine (60-75% yields) or 1,4-diazepane (71% yield) ring systems under Mitsunobu conditions. For some substrates addition of Et(3)N.HCl encouraged regioselective cyclisation through the secondary amine leading to aziridine ring systems. 相似文献
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V. V. Sharutin O. K. Sharutina L. P. Panova T. P. Platonova A. P. Pakusina V. K. Bel'skii 《Russian Journal of General Chemistry》2002,72(2):229-231
Tri-p-tolylantimony reacts with p-toluenesulfonic acid in the presence of benzoyl peroxide (1 : 2 : 1 molar ratio) in ether to give tri-p-tolylantimony ditosylate in 91% yield. According to X-ray diffraction data, the central antimony atom has the trigonal bipyramidal coordination with the axial location of the tosyl groups. The Sb-O bond lengths are 2.07(2) and 2.17(2) Å; Sb-C bond lengths, 2.08(3), 2.13(3), and 2.13(3) Å; and OSbO bond angle, 175.6(7)°. 相似文献
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在对甲苯磷酸存在下,采用1,1-二[4-(N,N-二取代氨基)苯基]乙烯(3)和四氯苯酐在乙酸酐溶液中的缩合反应合成了3,3-二{2,2-二[4-(N,N-二取代氨基)苯基]乙烯基}-4,5,6,7-四氯-2-苯并[c]呋喃酮(4),产率89~93%。3由4,4'-二(N,N-二取代氨基)二苯甲酮(1)与甲基碘化镁进行Grignard反应的产物经水解再脱水制得,产率85%~88.5%(以1为基准)。 相似文献