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研究了以2-羟基-4-甲氧基苯甲醛和2-氨基-6-甲基吡啶为原料合成新型席夫碱化合物5-甲氧基-2-[(E)-(6-甲基吡啶-2-亚氨基)甲基]苯酚的方法。当2-羟基-4-甲氧基苯甲醛与2-氨基-6-甲基吡啶摩尔比为1∶1.6,反应时间为6 h,反应温度为75℃时,反应产率最高。采用元素分析、UV-Vis、IR、1H NMR、X-射线单晶衍射等方法进行结构表征。该化合物为单斜晶系,空间群P21/c,a=1.1886(3)nm,b=0.65948(16)nm,c=1.6897(4)nm,β=108.505(3)°,V=1.2560(5)nm3,Dc=1.281 g·cm-3,Z=4,F(000)=512,μ=0.087 mm-1,R1=0.0477,wR2=0.1342。通过π···π堆积和分子内氢键O2-H2···N1、C8-H8A···N2形成较稳定的晶体结构,并具有蓝色荧光。 相似文献
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报道了从3-甲基-2-氨基苯甲酸出发一锅三步合成2-氨基-N,3-二甲基-5-卤代苯甲酰胺的方法.3-甲基-2-氨基苯甲酸(1)与固体光气反应生成中间体8-甲基-2H-3,1-苯并噁嗪-2,4(1H)-二酮(2),化合物2与甲胺水溶液发生胺解反应生成2-氨基-N,3-二甲基苯甲酰胺(3),3再与氯代丁二酰亚胺(NCS)、溴代丁二酰亚胺(NBS)或碘代丁二酰亚胺(NIS)发生芳香亲电取代反应生成目标产物2-氨基-N,3-二甲基-5-卤代苯甲酰胺(4~6).整个反应过程不需分离中间产品,最终产物经减压浓缩除去有机溶剂后,直接从水中析出针状晶体,总收率达到87%~94%,较文献报道的分步法收率提高30%以上.该方法工艺操作简单、反应条件温和、反应时间短、收率高,是一条环境友好的绿色合成路线. 相似文献
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丁烯基环戊二烯基稀土氯化物;1-甲基-1-丙基-3-丁烯基环戊二烯基稀土二氯化物的合成 相似文献
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以2,4-二甲基-6-叔丁基苯酚、多聚甲醛和三氯氧磷为原料,在四氯化碳溶剂中合成了6-叔丁基-3-氯甲基-2,4-二甲基苯酚并确定较佳的工艺条件,分别考察了物料配比、反应温度、反应时间和相转移催化剂用量对反应收率的影响。确定较佳工艺为:在四氯化碳溶剂中,反应温度为40℃,2,4-二甲基-6-叔丁基苯酚用量为60 g,多聚甲醛12 g,浓盐酸30 g,相转移催化剂4 g,三氯氧磷40 g。在上述条件下,6-叔丁基-3-氯甲基-2,4-二甲基苯酚的收率为95%,纯度>99%(HPLC面积归一化法),产品结构经IR、MS和~1H-NMR表征。 相似文献
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报道了一种分离甲苯、2-甲基噻吩和3-甲基噻吩的方法。通过氯化反应将沸点非常接近的甲苯、2-甲基噻吩和3-甲基噻吩转化为沸点相差较大的甲苯(111℃)、2-氯-5-甲基噻吩(155℃)和2,5-二氯-3-甲基噻吩(185℃),通过对比实验获得氯代反应的最佳条件为:2-甲基噻吩和3-甲基噻吩与磺酰氯的投料比1∶1. 75,反应温度65℃,反应时间2 h。通过精馏将三者分离并提纯,得到甲苯、高附加值的2-氯-5-甲基噻吩和2,5-二氯-3-甲基噻吩产品;通过催化还原反应将2-氯-5-甲基噻吩和2,5-二氯-3-甲基噻吩分别还原为2-甲基噻吩和3-甲基噻吩,达到完全分离、提纯的目的。 相似文献
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建立了工业苯酚中有机杂质的固相微萃取-气相色谱(SPME-GC)分析方法。实验考察了SPME萃取温度和萃取时间的影响,同时也优化了热解吸时间。优化后的萃取温度为20 ℃,萃取时间为10 min,热解吸时间为30 s。使用此法对工业苯酚样品中的两种主要有机杂质进行了分析检测,结果表明: 2-甲基苯并呋喃和2,4-二苯基-4-甲基-1-戊烯分别在0.05~1.06 mg/L和0.05~0.99 mg/L范围内线性关系良好(r2分别为0.990和0.992),检出限分别为0.5和1.6 μg/L。在0.1 mg/L的添加水平下,2-甲基苯并呋喃和2,4-二苯基-4-甲基-1-戊烯的回收率分别为104%和113%。该方法具有简单、快速、灵敏度高等优点,适合于工业苯酚中这两种主要痕量有机杂质的准确定量分析。 相似文献
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以2-氨基-2-甲基-丙醇为脂肪酸的化学修饰试剂,气相色谱一电子轰击质谱(GC-EI MS)分析葵子油脂肪酸。2-氨基-2-甲基-丙醇将脂肪酸羧基修改为含氮杂环,使在EI源中避免了链烯基中碳碳双键的移动。解析了葵子油脂肪酸2-氨基-2-甲基-丙醇化学修饰产物的EI质谱图,讨沦了烯酸中碳碳双键的定位规则,确定了葵子油脂肪酸中碳碳双键的位置。鉴定出葵子油6种脂肪酸,不饱和脂肪酸相对含量为89.41%,其中人体必需脂肪酸9,12-十八碳二烯酸含量占65.30%。本方法为不饱和脂肪酸中双键的定位提供了新的技术手段。 相似文献
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R. R. Gataullin F. F. Minnigulov A. A. Fatykhov L. V. Spirikhin I. B. Abdrakhmanov 《Russian Journal of Organic Chemistry》2002,38(1):31-37
Reactions of substituted 2-(1-methyl-2-butenyl)anilines with iodine result in cyclization and formation of 3-iodo-1,2,3,4-tetrahydroquinolines; N-methylsulfonyl-2-(1-methyl-2-butenyl)anilines give rise exclusively to the corresponding 2-(1-iodoethyl)-3-methyl-2,3-dihydroindoles. 相似文献
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Three new humulone derivatives have been isolated and identified as: 3,4-dihydroxy-2-(3-methyl-2-butenyl)-4-(4-methyl-3-pentenoyl)-2-cyclopentenone (6);4-ethanoyl-3,4-dihydroxy-2-(3-methyl-2-butenyl)-2-cyclopentenone (7) and 3,4-dihydroxy-2-(3-methyl-2-butenyl)-2-cyclopentenone (8), respectively. They arise by deacylation of anti-isohumulone (3a), which is formed from humulone (1a) following an isomerization with ring contraction in opposite direction than the usual one producing isohumulones (2a). 相似文献
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Tetsuji Kametani Kazuo Kigasawa Mineharu Hiiragi Nagatoshi Wagatsuma Tuneo Uryu Hideo Sugi 《Journal of heterocyclic chemistry》1973,10(1):27-29
Treatment of 1,2,5,6-tetrahydro-2-(4-hydroxy- and/or 4-methoxybenzyl)-3,4-dimethyl-I-(3-methyl-2-butenyl)pyridines (IV and V) and 2-(4-methoxybenzyl)-3,4-dimethyl-1-(3-methyl-2-butenyl)-4-piperidinol (X) with acid afforded 9-(4-hydroxy- and/or 4-methoxybenzyl)-4,4,5,6-tetramethyl-1-azabicyelo[3,3,1]non-6-ene (XIII and XIV). In contrast, the corresponding 1-allyl-substituted derivatives VI, VII, and XI were converted into the expected 3-allyl-1,2,3,4,5,6-hexahydro-8-hydroxy- and/or 8-methoxy-6,11-dimethyl-2,6-methano-3-benzazocine (II and III). 相似文献
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Pelly SC Govender S Fernandes MA Schmalz HG de Koning CB 《The Journal of organic chemistry》2007,72(8):2857-2864
The first enantioselective synthesis of the 2-isopropenyl-2,3-dihydrobenzofuran skeleton of tremetone and hydroxytremetone from (E)-4-(2-hydroxyphenyl)-2-methyl-2-butenyl methyl carbonate and (E)-4-(2,6-dihydroxyphenyl)-2-methyl-2-butenyl methyl carbonate, respectively, is described. The key step is a catalytic palladium-mediated reaction in the presence of the chiral Trost ligand. 相似文献
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6-(3-Methyl-but-2-enyl)-1,3-dihydro-indol-2-one, annonidine F [3-[6-(3-methyl-but-2-enyl)-1H-indolyl]-6-(3-methyl-but-2-enyl)-1H-indole], 1H-indole-5-carbaldehyde, 6-(3-methyl-2-butenyl)-1H-indole, 6-(3-methyl-buta-1,3-dienyl)-1H-indole, 6-(4-oxo-but-2-enyl)-1H-indole and 3-geranylindole were isolated from Monodora angolensis (Annonaceae) while 3-(1,1-dimethyl-but-2-enyl)-5-(3-methyl-but-2-enyl)-1H-indole (caulidine A), 4-[3-(1,1-dimethyl-but-2-enyl)-1H-indol-5-yl]-but-3-en-2-one (caulidine B), 5-(3-methyl-2-butenyl)-1H-indole and 5-(3-methylbuta-1,3-dienyl)-1H-indole were obtained from Isolona cauliflora (Annonaceae); structural determination by spectroscopic analysis. Some of the prenylindoles had antifungal and antimalarial activities. 相似文献
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Tetsuji Kametani Kazuo Kigasawa Mineharu Hiiragi Fumio Satoh Setsu Saito Hideo Sugi Tsuneo Uryu 《Journal of heterocyclic chemistry》1972,9(5):1057-1059
The configuration of the quaternary ammonium salts (Va and Vb) from 3-benzyl-1,2,3,4,5,6-hexahydro-8-hydroxy-6,11-dimethyl-2,6-methano-3-benzazocine. (II) and 3-methyl-2-butenyl bromide was determined spectroscopically. Moreover, configurational studies on 3-benzyl (VIa and VIb) and 3-(3-methyl-2-butenyl)benzazocinium bromides (VIIa and VIIb) were also achieved. 相似文献
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Microbial transformation of xanthohumol using the culture broth of Cunninghamella echinulata NRRL 3655 afforded (2S)-8-[4"-hydroxy-3"-methyl-(2"-Z)-butenyl]-4',7-dihydroxy-5-methoxyflavanone (5) and (2S)-8-[5"-hydroxy-3"-methyl-(2"-E)-butenyl]-4',7-dihydroxy-5-methoxyflavanone (6). Xanthohumol (1) and flavanone 6 as well as (E)-2"-(2"'-hydroxyisopropyl)-dihydrofurano[2",3":4',3']-2',4-dihydroxy-6'-methoxychalcone (2), (2S)-2"-(2"'-hydroxyisopropyl)-dihydrofurano[2",3":7,8]-4'-hydroxy-5-methoxyflavanone (3) obtained with Pichia membranifaciens showed antimalarial activity against Plasmodium falciparum. 相似文献
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Graziano Guella Ines Mancini Antonio Guerriero Francesco Pietra 《Helvetica chimica acta》1985,68(5):1276-1282
A mixture of sponges of the East Pyrenean Mediterranean is shown to contain the known sponge products longifolin ( 1 ), avarol ((+)- 3 ), and avarone ( 4 ) and the terrestrial-plant product sesquirosefuran ( 2 ), besides to the new furano-sesquiterpenoids tavacfuran (= 3-methyl-2-[(3′Z)-3′-methyl-4″-methyl-2″-furyl-3′-butenyl]furan; ( 5 ) and tavacpallescensin (= 5,10-dihydro-6,9-dimethyl-4H-benzo[5,6]cyclohepta[1,2-b]furan; 6 ) and the new furano-butenolide sesquiterpenoids tavacbutenolide-1 (= (±-4-ethoxy-2-methyl-4-)[(2′E)-2′-methyl-4′-(3″-methyl-2″-furyl)-2′-butenyl]-2-buten-4-olide; (±)- 7 ) and tavacbutenolide-2 (= (±)-4-ethoxy-3-methyl-4-[2′E)-3′-methyl-4′-(4″-methyl-2″-furyl)-2′-butenyl]-2-buten-4-olide; (±)- 8 ). Structural assignments are based on NMR data and on the synthesis of the (E)-isomer of 5 . The sponge Dysidea tupha of the same area is also shown to contain the two sesquiterpenoids ent-furodysinin ((?)- 14 ), which is enantiomeric to a product of a Dysidea sp. of Australian waters, and tuphabutenolide ((+)- 15 ). 相似文献
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Two naturally occurring 6-substituted indoles, 6-(3-methylbuta-1,3-dienyl)indole (2) and 6-(3-methyl-2-butenyl)indole (5), were synthesized by using an advanced Fischer indolization of a 2-methoxyphenylhydrazone derivative. 相似文献