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1.
以2-溴-3,3,3-三氟丙烯(1)为原料,经卤素-镁交换反应制得中间体三氟异丙烯基格氏试剂(2);2分别与CO2,正丁醛,苯甲醛和苯甲酰氯反应合成了2-三氟甲基丙烯酸(3a),2-三氟甲基-1-己烯-3-醇(3b),1-苯基-2-三氟甲基-2-丙烯-1-醇(3c)和1-苯基-4-三氟甲基-4-丁烯-1-酮(3d),其中3d为新化合物,其结构经1H NMR,13C NMR,IR,MS和元素分析表征。考察了交换试剂、物料比、温度和反应时间对3a产率的影响。在最优反应条件[以i-Pr Mg Br/Li Cl为交换试剂,1 50 mmol,n(2-溴丙烷)∶n(1)=1.25∶1.00,于-60℃反应2 h]下,3a收率64.3%。 相似文献
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以对氨基苯磺酰胺、丙烯酰氯(或甲基丙烯酰氯)为原料合成了N-[4-(磺酰胺)苯基]丙烯酰胺(ASPAA)和N-[4-(磺酰胺)苯基]甲基丙烯酰胺(ASPMAA),其结构经^1H NMR,IR和元素分析表征。合成ASPAA的最佳条件:对氨基苯磺酰胺13.76g(80mmol),n(对氨基苯磺酰胺):n(丙烯酰氯)=1.0:1.1,n(丙烯酰氯):n(NaHCO3):1.00:1.14,0℃~2℃反应3h,反应液倾入10倍体积的的甲醇-水[V(甲醇):V(水)=1:10]中析出产物,收率在60%以上。合成ASPMAA的最佳条件:对氨基苯磺酰胺6.88g(40mmol),n(对氨基苯磺酰胺):n(甲基丙烯酰氯)=1.00:1.05,n(三己胺):n(甲基丙烯酰氯):1.0:1.0,在0℃~2℃滴加甲基丙烯酰氯后先在室温下反应1h,然后在60℃反应1h,反应液倾入700mL石油醚中析出产物,收率50%~60%. 相似文献
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以3,5-二甲基苯酚为原料,经4步反应合成了1,1’-【{5-[3-(乙酰硫基)丙氧基]-1,3-亚苯基}双(亚甲基)】双{[(4,4’-联吡啶)-1-鎓]}二六氟磷酸盐(4);4与1,4-二溴甲基苯和萘模板在低温反应制得含硫代乙酸酯的缺电子环蕃(5);5经连续萃取及离子交换除去萘模板合成了新型含硫代乙酸缺电子环蕃——5,13,20,27-四氮杂七环[25,2,2,22,5,17,11,213,16,217,20,222,25]四十-9-(1-丙基硫代乙酸酯)氧-1(28),2,4,7,9,12,14,16,18,21,23,26,29,31,33,35,37,39-十八烯四六氟磷酸盐(6),其结构经1H NMR和13C NMR表征。 相似文献
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以1,6-二甲酰基环庚三烯为原料通过10π电子环化反应等3步反应制备了3-溴代-1,6-亚甲基桥[10]轮烯,通过3-溴代-1,6-亚甲基桥[10]轮烯的碱诱导的偶联反应,简便地合成3,3′-联-1,6-亚甲基桥[10]轮烯,并用NMR,MS等波谱进行了表征。 相似文献
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以9-芴甲酸为起始原料经亲核取代反应和N-酰基化反应制得N-(2,2,2-三氟乙基)-9-(4-溴丁基)-9H-芴基-9-甲酰胺(4);4'-(三氟甲基)-[1,1'-联苯]-2-羧酸与N-叔丁氧羰基-4-氨基哌啶反应制得中间体N-(1-叔丁氧羰基哌啶-4-基)-4'-(三氟甲基)-[1,1'-联苯]-2-甲酰胺(7);7在4 mol·L-1HCl二噁烷溶液中脱除保护基制得N-(哌啶-4-基)-4'-(三氟甲基)-[1,1'-联苯]-2-甲酰胺盐酸盐(8);8与4在K2CO3作用下反应制得洛美他派(9);9与甲磺酸经成盐反应合成了甲磺酸洛美他派,总收率36.4%,其结构经1H NMR,IR和HR-ESIMS确证。 相似文献
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以6,7-十二烷二酮(或1,2-环烷基二酮)和3-碘-2-碘甲基-1-丙烯为原料,铟粉为催化剂,在水相中经烯丙基化反应合成了4个新型的单烯丙基化产物[7-羟基-7-(2-碘甲基-烯丙基)-十二烷-6-酮和2-羟基-2-(2-碘甲基-烯丙基)-环烷酮]和3个新型的双烯丙基化产物{4-亚甲基-1,2-二戊基-1,2-环戊二醇,2-羟基-2-[2-(1-羟基-2-羰基-环癸基甲基)-烯丙基]-环癸酮和2-羟基-2-[2-(1-羟基-2-羰基-环十二基甲基)-烯丙基]-环十二烷酮},其结构经1H NMR,IR和HR-MS表征。 相似文献
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The Ni-catalyzed cross-coupling of 2-bromo-3,3,3-trifluoropropene and aryl Grignard reagents was investigated. When NiCl2(PPh3)2 was used as a catalyst, the highest yield of α-trifluoromethylstyrene (89%) from 2-bromo-3,3,3-trifluoropropene and PhMgBr was obtained in 1,3-dimethyl-2-imidazolidinone at 50 °C for 30 min. Various α-trifluoromethylstyrene derivatives could be produced in satisfactory yields by NiCl2(PPh3)2-catalyzed coupling using aryl Grignard reagents. 相似文献
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The reaction of 3,3,3-trifluoropropene with N-bromosuccinimide in acetic acid at 65—70 °C affords 3-acetoxy-2-bromo-1,1,1-trifluoropropane. When treated with an alkali, the latter is readily converted into (trifluoromethyl)oxirane. 相似文献
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在Pd(PPh~3)~4/CuI催化下和使用1mol的NEt~3作碱和THF作溶剂,(Z)-3-碘-3-三氟甲基-1-芳基烯丙醇(1)与末端炔烃(3)反应得到正常的偶联产物5。当以NEt~3作碱和溶剂,Pd(PPh~3)~4/CuI催化1与3的交叉偶联反应生成化合物4。4为正常偶联化合物5在NEt~3存在下双键发生重排反应的产物。 相似文献
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P. Veeraraghavan Ramachandran Kamlesh J. Padiya 《Journal of fluorine chemistry》2007,128(10):1255-1259
Bromination of 3,3,3-trifluoropropene in 20% oleum, followed by treatment with acetic acid furnishes 2-bromo-3,3,3-trifluoropropyl acetate in quantitative yield, which upon acid hydrolysis and cyclization with alkali affords 3,3,3-trifluoropropene oxide (TFPO) in 63% overall yield. 相似文献
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Peter Cooper Roy Fields Robert N. Haszeldine Gordon H. Mitchell Shmaiel N. Nona 《Journal of fluorine chemistry》1982,21(3):317-327
Tris(trifluoromethyl)phosphine and ethylene reacted efficiently under u.v. irradiation to give 3,3,3-trifluoropropylbis(trifuomothyl) phosphine in good yield. With vinyl fluoride, vinylidene fluoride, and propene the reaction was regioselective rather than regiospecific, and the yield of 1:1 adduct was low. In these reactions, and in those with vinyl chloride, but-1-ene, and hexafluoropropene, in which only traces of 1:1-adduct could be detected, the bulk of the olefin and of the phosphine was recovered, and numerous by-products consistent with radical intermediates were identified. With propyne, 1,1,1-trifluoro-3-bis(trifluoromethyl)phosphino-cis-but-2-ene was obtained in moderate yield, but no reaction occurred between the phosphine and either but-2-yne or hexafluorcbut-2-yne. Tris(trifluoromethyl)phosphine oxide did not form an adduct with ethylene, tetrafluoroethylene, or propyne.Bis(trifluoromethyl)phosphine and dimethylphosphine both reacted readily under u.v. irradiation with 3,3,3-trifluoropropene, the phosphinyl radical attacking the terminal carbon in each case. 相似文献
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Copper-Catalyzed Synthesis of 5-Aryl-6-(Trifluoromethyl)-2,3-Dihydropyrazolo[1,2-a]Pyrazol-1(5H)-One
Xinyu Zhang Hui Wang Dr. Lili Xie Chenhui You Dr. Xiaoyan Han Prof. Dr. Zhiqiang Weng 《化学:亚洲杂志》2021,16(18):2669-2673
An efficient protocol for the synthesis of 5-aryl-6-(trifluoromethyl)-2,3-dihydropyrazolo[1,2-a]pyrazol-1(5H)-one derivatives through a copper-catalyzed [3+2]-cycloaddition of azomethine imines with 3,3,3-trifluoropropyne (generated in situ from dehydrobromination of 2-bromo-3,3,3-trifluoropropene under base conditions) is developed. The advantages of this transformation are the broad substrate scope and the good functional group compatibility. The subsequent oxidation and nucleophilic substitution/aromatization provide a new approach to 4-trifluoromethylated pyrazol-1-yl propanoic acids. 相似文献
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《Tetrahedron letters》2017,58(34):3377-3379
A series of 1-sulfonyl-1-trifluoromethyl allenes were prepared for the first time from commercial available 2-bromo-3,3,3-trifluoropropene. Cycloaddition reaction of these trifluoromethylated allenes with nitrones occured readily under mild conditions, giving the corresponding trifluoromethylated isoxazolidines in high yields. 相似文献
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Wojciech Dmowski 《Journal of fluorine chemistry》1985,29(3):287-296
1-Phenyl-2-chloro-3,3,3-trifluoropropene and 1-phenyl-l,2-dichloro- 3,3,3-trifluoropropene were prepared from 1-phenyl-3,3,3- -trifluoropropene by a chlorination-dehydrochlorination sequence. Intermediate 1-phenyl-l,2-dichloro-3,3,3-trifluoropropane and 1-phenyl-1,2,2-trichloro-3,3,3-trifluoropropane were also isolated. All compounds were characterised by elemental analysis, boiling points, 1H and 19F NMR spectra. 相似文献
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Trifluoromethylated polyfunctionalized cyclopropanes were obtained in high stereoselectivity by reacting 2-bromo-3,3,3-trifluoropropene (BrTFP) with active methylenes. This novel method was further applied to the synthesis of (+/-)-trans-trifluoronorcoronamic acid. 相似文献
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Takeo Taguchi Ginjiro Tomizawa Akihiro Kawara Masaharu Nakajima Yoshiro Kobayashi 《Journal of fluorine chemistry》1988,40(2-3):171-182
Reaction of 1-phenylsulfonul-3,3,3-trifluoropropene(1) with carbonyl-stabilized enolate anions smoothly proceeded to give the addition products(7) in good yield while with an alkyl-lithium or Grignard reagent the formation of the vinyl anion(8) was one of the reaction pathways. Reaction of 1 with the chiral nucleophiles(11, 16) was carried out to give the functionalized trifluoromethylated compounds(13, 7b) in 4-43% ee 相似文献