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二氯化合物

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In this paper, we designed and synthesized a molecule of compound 1, 2-(benzooxazol-2-yl)-5-4-(3-(benzothiazol-2-yl) phenylamino-6--1,3,5-triazin-2-ylaminophenol, which can only assembled into an organogel upon a short irradiation with ultrasound in toluene-methanol mixed solvent. DSC, XRD and IR were used to detect the properties and mechanisms of the organogel.

本论文中,我们设计合成了一个有机小分子化合物1,4-氨基(2-羟基苯基)苯并噁唑3-氨基苯基苯并噻唑二辛基胺缩三聚氯嗪,研究发现,在甲苯/甲醇=1:2的混合溶剂中,只有利用超声才能使之形成凝胶,加热冷却的方法不能形成凝胶,而形成针状结晶。

In order to check the corresponding compound at 31P NMR –45.4 ppm, stable pentacoordinate spirobicyclic 2-phenoxy-1,3-phenylene-dioxo-1,3,2-iminoacetoxyphosphoranes were synthesized through a new and efficient method whereby phosphorus pentachloride was displaced stepwise by catechol, N,O-bisamino acid and phenol, or catechol, phenol and N,O-bisamino acid, their 31P NMR chemical shifts are at about 31P NMR –45.0 ppm, the results showed that the compound 4 at 31P NMR –45.4 ppm was pentacoordinate phosphorane containing amino acid residue.

采用磷谱跟踪来研究上述成肽反应机理。例如在氮气保护下,0.1mmol O,O-亚苯基磷酰氯(1)和0.15mmol N,O-二苯丙氨酸(2)苯溶液加入0.6ml核磁管中,混合均匀,反应过程用磷谱检测。反应1分钟后,起始原料1(δp=19ppm)很快转变成N-磷酰苯丙氨酸的三甲基硅基酯(3)(δp=19.8ppm),在8分钟内,3完全转变成苯丙氨酸磷烷4(δp =-45.4ppm),同时出现环磷三酯(6)(δp=3.5ppm)。随着反应的进行,对应于化合物4的峰逐渐变小,而6逐渐变大。

A new imidazolinyl intermediate is prepared from phenylacetic acid and diethylenetriamine firstly, and then they react with the solution of sodium chloroacetate into the imidazolinyl quaternary ammonium salt.

以二甲苯为溶剂,苯乙酸和二乙烯三胺为原料,经酰胺化和环化脱水合成了新型咪唑啉化合物,并用氯乙酸钠溶液对其进行改性得到了苯乙酸咪唑啉季铵盐。

A reduction-coupling-etherification reaction between aromatic aldehydes or ketones (1) and alcohols ( 2 ) to yield corresponding diether ( 3 ) of pinacol in the presence of tin and chlorotrimethylsilane.

在三甲基氯硅烷、四氢呋喃体系中,芳香醛、酮和醇在金属锡的作用下发生还原-偶联-醚化反应生成相应的频那醇二醚类化合物。

Two novel pyrazolone derivatives 2-ethylamino-6H-5-(1-phenyl-3-methyl/phenyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine (PMCP-ETSC/DPCP-ETSC) containing NNS six-membered heterocycles were synthesized by the condensation reaction of 1-phenyl-3-methyl/phenyl-4-chloroacetyl-pyrazolone-5 with 4-ethyithiosemicarbazide. The title compounds were characterized by elemental analysis, IR, 1H NMR, 13C NMR and single-crystal X-ray diffraction.

利用1-苯基-3-甲基/苯基-4-氯乙酰基-吡唑啉酮-5与4-乙基氨基硫脲发生缩合反应,生成了2个新的双杂环化合物2-乙氨基-6H-5-(1-苯基-3-甲基/苯基-5-吡唑啉酮-4-基)-1,3,4-噻二嗪(PMCP-ETSC/DPCP-ETSC),并对其进行元素分析、红外光谱、核磁共振表征和晶体结构分析。

Methods 4-Hydroxy- benzonitrile was treated with sodium hydrogen sulfide and anhydrous magnesium chloride in dimethyl formamide to give thioamide, which was then directly cyclized with ethyl 2-chloroacetoacetate without separation to give ethyl 2-(4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(2) in one-pot; then 2 was formylated with Duff reaction adopting hexamethylenetetramine in trifluoroacetic acid to give ethyl 2-(3-formyl-4-hydroxyphenyl)-4-methylthiazole-5-carboxylate(3); finally, the target compound was obtained by the treatment of 3 with hydroxylamine hydrochloride and sodium formate in formic acid.

采用&一勺烩&方法,以4-羟基苯甲腈为起始原料,首先与硫氢化钠和无水氯化镁在N,N-二甲基甲酰胺中反应,所得中间体不经分离,直接加入2-氯乙酰乙酸乙酯进行环合反应,得到2-(4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(2);然后通过六亚甲基四胺/三氟乙酸进行Duff反应,得到2-(3-甲酰基-4-羟基)苯基-4-甲基-5-噻唑甲酸乙酯(3);再经盐酸羟胺/甲酸/甲酸钠体系脱水得到目标化合物。

The title compounds were prepared using chlororesorcinol and trimellitic anhydride as the starting materials in seven steps, with fine overall yields.

以氯代间苯二酚和苯三酸酐为起始原料经7步反应得到了目标化合物,产率良好。

In this article,a non-carcinogenic dye intermediate 4-aminodianiline-2-sulfonic acid is synthesized from 4-nitro-1-chlorobenzen through sulfonation,condensation and reduction.

针对联苯胺作为合成染料的重要中间体已被确认为致癌物的情况,以对硝基氯苯为原料,经磺化、缩合、还原,合成了一种无致癌性并取代联苯胺的双胺化合物染料中间体4-氨基二苯胺-2-磺酸,利用红外光谱、差热和氢谱核磁对其性质进行了表征。

For the α-arylation of ethyl acetoacetate, the product was α-aryl ethyl acetoacetates, rather than ethyl α-arylacetates which are the major products in other catalytic systems.

较为惰性的氯代芳烃在Pd2/L1的催化下,也能够跟1,3-二羰基化合物发生α-芳基化反应。

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