共查询到20条相似文献,搜索用时 93 毫秒
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根据Kornblum反应,采用二甲基亚砜(DMSO)氧化E-1-乙酰氧基-4-氯-3-甲基-2-丁烯(ACMB)合成E-4-乙酰氧基-2-甲基-2-丁烯-1-醛(AMBA)。在实验过程中,采用气相色谱跟踪,研究了反应时问、反应温度和催化剂用量等因素对主副产物收率的影响并确定了较佳反应条件;反应时间24h,反应温度80℃,原料缓慢滴加,KH2PO4:K2HPO4:ACMB=0.14:1.27:1(摩尔比),催化剂用量与原料ACMB比为0.12:1(摩尔比)。同时,对从未报道过的副产物E-1-乙酰氧基-4-甲巯基-3-甲基-2-丁烯(AMMB)进行了结构鉴定,并推测了其形成机理。 相似文献
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2,3-二甲氧基-5-甲基-6-(3-甲基-2-烯-1-丁基)-1,4-苯酚的合成及其副产物的研究 总被引:1,自引:0,他引:1
2,3-二甲氧基-5-甲基-1,4-苯酚与2-甲基丁烯醇在BF3OEt2的催化下进行傅-克烷基化反应合成2,3-二甲氧基-5-甲基-6-(3-甲基-2-烯-1-丁基)-1,4-苯酚。对鲜见文献报道的副产物2,2,5-三甲基-3-氢-6-羟基-7,8-二甲氧基-苯并吡喃进行了结构鉴定并推测了其形成机理,在原料辅酶Q0、甲基丁烯醇和BR的配比为1:1.5:0.19(摩尔比),反应温度45℃,滴加时间30min,反应时间2h的条件下收率达90.24%。 相似文献
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李云霞 《精细与专用化学品》2010,18(6):39-41
以正丁酸乙酯和草酸二乙酯为主要原料,合成了香料化合物3-乙基-2-羟基-2-环戊烯-1-酮。首先由正丁酸乙酯和草酸二乙酯经Claisen缩合生成2-乙基-3-羰基-丁二酸乙酯,其与丙烯酸乙酯发生Michael加成,随后Dieckmann酯缩合得到5-乙基-3,5-二乙酯基-2-羟基-2-环戊烯-1-酮,然后经水解脱羧获得3-乙基-2-羟基-2-环戊烯-1-酮。初步考察并优化了各步反应的工艺条件,产品总收率达44.46%。 相似文献
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2-(2-氯-丙酰基)-6-氯-9-乙酰基-咔唑是一种风湿类药物的中间体,本文研究了以咔唑和醋酐等为原料,经过酰化→丙酰化→氯化反应,合成2-(2-氯-丙酰基)-6-氯-9-乙酰基-咔唑的技术。研究了不同反应条件对反应收率的影响,得出最佳方案。总收率可达51%。 相似文献
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本文阐述了1,2-萘醌-2-重氮基-5-磺酰氯的生产和废水处理,并通过络合萃取法进行废水处理,回收了原料1,2-萘醌-2-重氮基-5-磺酸钠。 相似文献
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提出了对氯-r-溴丙苯的合成方法,以对氯氯为原料制取对氯苄基氯化镁,通过镁过量解决了在四氢呋喃中的偶联问题,提高了格氏试验剂的收率,此格氏试剂与环氧乙烷反应得到氯-r-苯丙醇,然后在三氯甲烷助溶剂作用下,与过量的氢溴酸反应得到对氯-r-溴丙苯,文中优化得出了最佳合成条件,为工业化生产提供了理论依据。 相似文献
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以吲哚-4-甲醛、对甲基苯肼和对氯苯胺为原料,合成了1-(4-甲苯基)-3-(4-吲哚基)-5-(4-氯苯基)甲臢。经红外、核磁和质谱等波谱鉴定了目标分子的结构,并测定了它的氧化还原电位值。 相似文献
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The synthesis of 4-thiazoline 2-iminium sulfinates ( 3 ) is described. From the salts 3 and NBS the 2-(arylsulfonylimino)-4-thiazolines ( 4 ) were formed, which have also been prepared by oxidation of 2-(arylsulfenylimino)-4-thiazolines ( 5 ) and by reaction of the arylsulfonyl chlorides ( 6 ) with 2-imino-4-thiazolines ( 2 ). The treatment of 5 with NBS (or NIS) in dry solvents results in 2-(arylsulfenylimino)-5-bromo (or iodo)-4-thiazolines ( 7 ); in the presence of NaHCO3 2-(arylsulfonylimino)-5-bromo-4-thiazolines ( 8 ) are formed. 2-(Arylsulfinylimino)-4-thiazolines ( 10 ) have also been halo- genated in the same manner with NBS or NIS to give the products ( 11 ). 相似文献
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1-(3-氨基苯基)-3-(4-氨基苯基)-2-丙烯-1-酮的合成 总被引:4,自引:0,他引:4
以对乙酰氨基苯甲醛、间乙酰氨基苯乙酮为原料经两步反应合成具有光敏性能的1 (3 氨基苯基) 3 (4 氨基苯基) 2 丙烯 1 酮。通过优化实验得到最佳的合成工艺条件为:对乙酰氨基苯甲醛、间乙酰氨基苯乙酮在温度为0℃下,以乙醇为溶剂、氢氧化钠为催化剂,进行羟醛缩合反应3h。分离提纯后,加入盐酸溶液在100℃下水解3h,产物经重结晶提纯。总收率达到61 9%,较1998年的文献[6]提高39 3%。并对产物的结构进行了表征。 相似文献
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Palanisamy RAVICHANDIRAN Dhanaraj PREMNATH Samuel VASANTHKUMAR 《Frontiers of Chemical Science and Engineering》2015,9(1):46
A new series of 2-(4-(4-aminophenylsulfonyl)phenylamino)-3-(thiophen-2-ylthio)naphthalene-1,4-dione derivatives ( 3a-3n) were synthesized and characterized by spectral techniques. To understand the interaction of binding sites with bacterial protein receptor, the docking study was performed by the GLIDE program and compound N-(4-(4-(1,4-dioxo-3-(thiophen-2-ylthio)-1,4-dihydronaphthalen-2-ylamino)phenylsulfonyl)phenyl)-3-methylbenzamide ( 3b) exhibited good glide and E model scores of ?5.89 and ?94.90, respectively. Moreover among all the molecules studied including the standards used, namely Sparfloxacin (4.8 μg/mL) and Norfloxacin (no inhibition observed) for their antibacterial property, compound N-(4-(4-(1,4-dioxo-3-(thiophen-2-ylthio)-1,4-dihydronaphthalen-2-ylamino)phenylsulfonyl)phenyl)-4-nitrobenzamide ( 3e) exhibited the lowest minimum inhibitory concentration (MIC) value of 1.3 μg/mL against Proteus vulgaris. 相似文献
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E. Fanghnel J. U. Bauroth H. Hentschel F. Gußmann H. Alzyadi W. Ortmann 《Advanced Synthesis \u0026amp; Catalysis》1992,334(3):241-247
1,2,3-Triazabutadienes. XXII. Photochemistry of 1-(Carbmethoxy-aryl)- and 1-(Carboxy-aryl)-3-(3-alkyl-benzthiazolinyliden-(2))-triazenes as potential CEL-dyes 1-(Carbmethoxy-aryl)-3-(3-alkyl-benzthiazolinyliden-(2))-triazenes (ester-triazenes) ( 1 ) were synthesized by coupling of substituted 3-alkyl-2-imino-benzthiazolines-(1,3) with 2-, 3- and 4-carbmethoxy-benzenediazonium salts. The Z-isomers obtained can be transformed into the E-isomers 2 photochemically or by heating. In the presence of acids the E-ester-triazenes are protonated. From the E-ester-triazenes the potassium-salts ( 4 ) can be produced by alkaline ester hydrolysis. With hydrochloric acid the E-triazene-potassium salts ( 4 ) can be transformed into the protonated (at the N(1)-Atom) E-acid-triazenes ( 5 ). Their photochemical properties are identical with those of the protonated E-ester-triazenes ( 3 ). The 1-(carboxy-aryl)-3-(3-alkyl-benzthiazolinyliden-(2))-triazenes (E-acid-triazenes) ( 6 ) can be obtained from the protonated derivates by deprotonation in the presence of water. The photochemical behaviour of the E-acid-triazenes ( 6 ) and of the E-triazene-potassium-salts ( 4 ) depends on the position of the carboxy-group (2-position: photolysis, 3- and 4-position: photoisomerization). The uv/vis-spectroscopical and photochemical properties of the triazene-derivates in solution and in polymeric layers are discussed. 相似文献
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以4-甲氧羰基哌啶盐酸盐(1)和对三氟甲氧基苯甲酰氯(2)为起始原料,在三乙胺的作用下以92.7%的收率制得1-(4-三氟甲基苯甲酰基)-4-甲氧羰基哌啶(3);化合物(3)在羰基二咪唑与N,O-二甲基羟胺盐酸盐(4)作用下,以89.9%的收率制得1-(4-三氟甲氧基苯甲酰基)-4-(N-甲基-N-甲氧基羰基)哌啶(5);化合物(5)和4-甲氧基苯基溴化镁(6)偶联,以60.1%的收率制得化合物1-(4-三氟甲氧基苯甲酰基)-4-(4-甲氧基苯甲酰基)哌啶(7)。三步反应总收率50.0%。 相似文献
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