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乙酯基

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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。

Eight novel N,N′-naphthalene acyl substituted aromatic acylamino thiocarbamide s(Ⅱ1~Ⅱ8) were synthesized from aryl acylhydrazine and α-naphthalene acyl isothiocyanate, which was obtained by the reaction of potassium thiocyanate with α-naphthalene acyl chloride obtained from 2-naphthylacetic acid and thionyl chloride in anhydrous benzene.

通过α-萘乙酸和SOCl2在无水苯中反应制得α-萘乙酰氯,与硫氰酸钾反应生成α-萘乙酰基异硫氰酸酯,再与芳基酰肼进行加成反应,合成8种新型N,N′-萘乙酰基取代芳乙酰胺基硫脲类化合物(Ⅱ1~Ⅱ8)。

Methacryloyloxydecyl-2-thiouracil-5-carboxylate was synthesized from the reaction of thiouracil with diethyl ethoxymethylene malonate and ω-hydroxy-decyl-methacrylate.

以硫脲、乙氧基次甲基丙二酸二乙酯和甲基丙烯酸ω-羟癸酯为主要原料合成了一种新的粘接性单体10-甲基丙烯酰氧癸基-2-硫脲嘧啶-5-羧酸酯。

In addition, there were also some special aromatic substances such as 1-nonanol, hexanoic acid 2-hexenyl ester, propanoic acid 2-hexenyl ester, butanioc acid 3-hexenyl estertrans-2-hexenyl valerate, theaspirane, gerenylacetone, methyl benzoate and ethyl benzoate.

此外还含有一些少量的1-壬醇、己酸-2-己烯酯、丙酸-反-2-己烯酯、丁酸-反-3-己烯酯、戊酸-反-2-己烯酯、茶螺烷、香叶基丙酮、苯甲酸甲酯、苯甲酸乙酯和乙酸辛酯等。

Eight novel N,N′-naphthalene acyl substituted aromatic acylamino thiocarbamides(Ⅱ1~Ⅱ8) were synthesized from aryl acylhydrazine and α-naphthalene acyl isothiocyanate, which was obtained by the reaction of potassium thiocyanate with α-naphthalene acyl chloride obtained from 2-naphthylacetic acid and thionyl chloride in anhydrous benzene.

通过α-萘乙酸和SOCl2在无水苯中反应制得α-萘乙酰氯,与硫氰酸钾反应生成α-萘乙酰基异硫氰酸酯,再与芳基酰肼进行加成反应,合成8种新型N,N′-萘乙酰基取代芳乙酰胺基硫脲类化合物(Ⅱ1~Ⅱ8)。

Till today, we have extracted and purified alkaloids from from Macleaya Cordata, Chelidonium Majus L., Tripterygium Wilfordii Hook f., Sedum Sarmentosum Bunge, and obtained pure sanguinarine, ethoxysanguinarine, oxysanguinarine, chelidonine, chelerythrine, ethoxychelerythrine, chelilutine, chelirubine, protopine,α-allocryptopine,β-allocryptopine, coptisine, berberine, corysamine, bocconine; triptolide, tripdiolide, triptonide, wilforddine; N-methylisopelletierine, dihydro-N-methylisopelletierine, sarmentosin etc.

我们对博落回、白屈菜、雷公藤、垂盘草等天然植物进行了大量的提取和分离研究;并分离出了血根碱、乙氧基血根碱、氧化血根碱、白屈菜碱、白屈菜红碱、乙氧基白屈菜红碱、白屈菜黄碱、白屈菜玉红碱、原阿片碱、α-别隐品碱、β-别隐品碱、黄连碱、小檗碱、沙明碱、博落回碱,雷公藤内酯醇、雷公藤内酯二醇、雷公藤内酯酮、雷公藤碱,N-甲基异石榴皮碱、二氢- N-甲基异石榴皮碱、垂盘草甙等单体。

In order to investigate the mechanism for this reac-tion, methyl α-bromoacetate or ethyl α-bromoacetate as starting material was added to the solution of phenyl selenoamide in ethanol in 1∶1 or 2∶1 molar ratio under the neutral condition at room temperature. The results indicated that the same product bis or bis diselenide was formed. Byproduct ethyl benzoate was also separated.

为了研究该反应机理,选择α-溴代乙酸甲酯或α-溴代乙酸乙酯在无催化剂、中性条件下,乙醇溶液中与苯基硒代酰胺室温下反应,投料比为1∶1和2∶1,结果也都生成了同一类产物二甲氧羰基甲基二硒醚或二乙氧羰基甲基二硒醚,同时还分离得到了相应的副产物苯甲酸乙酯。

In order to investigate the mechanism for this reaction, methyl α-bromoacetate or ethyl α-bromoacetate as starting material was added to the solution of phenyl selenoamide in ethanol in 1:1 or 2:1 molar ratio under the neutral condition at room temperature. The results indicated that the same product bis or bis diselenide was formed. Byproduct ethyl benzoate was also separated.

为了研究该反应机理,选择α-溴代乙酸甲酯或α-溴代乙酸乙酯在无催化剂、中性条件下,乙醇溶液中与苯基硒代酰胺室温下反应,投料比为1:1和2:1,结果也都生成了同一类产物二甲氧羰基甲基二硒醚或二乙氧羰基甲基二硒醚,同时还分离得到了相应的副产物苯甲酸乙酯。

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。

Two series of polyurethane acrylate grafted acrylic resins (Acr-g-TPU-PETA and Acr-gPPU-PETA) self-emulsifying systems are obtained by grafting -NCO group modified polyurethane acrylates with acrylic copolymer prepared from n-butyl acrylate, styrene,βhydroxyethyl methacrylate and acrylic acid The self-emulsifying systems showed Newtonian fluidity with viscosity closed to that of water, the solid contents were around 30% The T〓 of 15~4℃ for dried film before photocuring favored film formation at room temperature DSC and DMA results showed that PU-PETA is compatible with acrylic resin in the grafted resin The TG and dTG curves for Acr-g-PU-PETA samples were substantially different from the corresponding blends, and the brodened dTG peaks for photocured grafted resin suggest that there might be multiple interactions among chain segments The photocued film of the grafted resins self-emulsifying system exhibited good overall properties with polyurethane acrylate grafts ranging from 30% to 50%, and Acr-g-TPU-PETA series showed better properties than Acr-gPPU-PETA series The adhesion of the photocured film was 1~2 grade, impact strength was 50kg-cm and flexibility was 1mm The Shore hardness and the adhesion of the film decreased markedly if PETA was replaced by HEMA as photoactive group due to the lower C=C double bond content in the grafted resin The polyhydroxy amine-linked thioxanthones photoinitiators can be evenly dispersed in self-emulsifying system without color spot appearing in the dried film The films photocured with IV〓~IV〓 generally exhibited higher Shore hardness, gloss and solventresistance than that cured with Irgacure 2959 and did not induce the rusting of the iron substrate Pigmenting with titanium oxide had no effect on the photocuring The polyhydroxy amine-linked thioxanthone IV〓 and IV〓 can be new candidates for the formulation of titanium oxide pigmented photocurable water-borne coatings for their pale-yellow appearance and slight interference with the color of the coatings WB 4759 with high water-solubility coalesced and separated from the dried resin film, and even induced the rusting of iron substrate.

以丙烯酸丁酯,甲基丙烯酸-β-羟乙酯,丙烯酸及苯乙烯合成厂丙烯酸共聚树脂,并与含-NCO端基的聚氨酯丙烯酸酯接枝反应,经水性化后,得到两个系列(Acr-g-TPU-PETA和Acr-g-PPU-PETA)各5个不同配比的丙烯酸树脂接枝聚氨酯丙烯酸酯自乳化体系,粘度与水相近,为牛顿流体,固含量30%左右。光固化前干燥涂膜的玻璃化转变温度在-15℃~4℃之间,有利于室温下成膜。DSC及DMA谱表明两种树脂基本相容。Acr-g-PU-PETA的热失重行为明显不同于共混材料,接枝样dTG峰明显宽化,表明接枝样中链段之间的相互作刚有多重性,丙烯酸树脂与聚氨酯之间有一定的相容性。接枝树脂自乳化体系光固化涂层的综合性能以聚氨酯丙烯酸酯成分为50%~30%者相对较好,且以Acr-g-TPU-PETA系列更理想。光固化膜的附着力为1~2级,冲击强度为50kg·cm,柔软性多为1mm。以HEMA代替PETA作为接枝树脂的活性基团,碳—碳双键密度太低,光固化膜交联点太少,硬度和附着力均较差。多羟基胺连硫杂蒽酮光引发剂能均匀分散于树脂自乳化体系和接枝树脂干膜中,不出现色斑,光固化膜肖氏硬度一般高于以Irgacure 2959为光引发剂的光固化膜,光泽度及耐丁酮溶剂性能均有所提高,不会诱导铁基生锈,钛白着色对光固化结果几乎没有影响。本论文所合成的多羟基胺连硫杂蒽酮光引发剂IV〓与IV〓为浅黄色,对光固化涂层的颜色干扰较小,为配制钛白着色光固化水性涂料提供了新的光引发剂。水溶性太强的WB 4759在干膜中易聚结析出,且对所附着的铁基有诱导锈蚀作用。

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