3，5－二氯－1－甲基－4－吡唑羧酸的制备

３，５－二氯－１－甲基－４－吡唑羧酸酯作为起始原料，用一步法制备了３，５－二氯－１－甲基－４－吡唑羧酸。     

2－丁氧基－5－（1，1，3，3－四甲基丁基）－苯硫酸的合成

以４－（１，１，３，３－四甲基丁基）－苯酚２为原料，通过３步合成了２－丁氧基－５－（１，１，３，３－四甲基丁基）－苯硫酚１。４－（１，１，３，３－四甲丁基）－苯酚２是由苯酚与二聚异丁烯（Ｄｉｉｓｏｂｕｔｙｌｅｎｅ）在硫酸存在下反应制得。３个化合物的结构以１ＨＮＭＲ予以表征。     

1，3－二氯－2－丁烯氯化产物的气相色谱分析

用气相色谱法测定１，３－二氯－２－丁烯的氯化产物，采用３０１釉化担体：阿皮松Ｌ：聚乙二醇－２０Ｍ－２－硝基对苯二甲酸＝１００：１０：０．８（质量比）的固定相填充柱分离了氯化产物中１６个组分。用色谱－质谱联用法鉴定这些组分为２，３，４－三氯－１－丁烯、２－甲基－３，３，３－三氯－１－丙烯、１，２，３，３－四氯丁烷、１，２，３，３，４－五氯丁烷等。用面积归一化法计算出了氯化产物中各组分含量。     

N1-(2-苯基-1,2,3-三唑-4-甲酰基)-吡唑类衍生物的合成

利用２－苯基－１,２,３－三唑－４－甲酰肼（１）分别与３－芳基偶氮乙酰丙酮（２）和３－芳基偶氮乙酰乙酸乙酯（３）在酸性条件下环化,制得１２个新的Ｎ１－（２－苯基－１,２,３－三唑－４－甲酰基（－３,５－二甲基－４－芳基偶氮吡唑（４）和Ｎ１－（２－苯革－１,２,３－三唑－４－甲酰基）－３－甲基－４－芳基偶氮－２－吡唑啉－５－酮（５）,用元素分析、ＩＲ、＾１ＨＮＭＲ和ＭＳ确定了它们的结构。     

2－吡唑啉类化合物光物理行为的研究──分子内两种电荷转移机制的竞争

２－吡唑啉类化合物光物理行为的研究──分子内两种电荷转移机制的竞争闫正林，吴世康（中国科学院感光化学研究所，北京１００１０１）关键词１，３，５－三芳基－２－吡唑啉，光诱导电荷转移，非水溶剂酸碱指示剂，荧光量子产率近年来，１，３，５－三芳基－２－吡唑啉...     

新芽前,芽后早期稻田除稗剂MY—100

新芽前、芽后早期稻田除稗剂ＭＹ－１００１理化性质结构式：ＯＮＨ３ＣＯＣＨ３ＣＨ３Ｃ１Ｃ１化学名称（ＩＵＰＡＣ）：３－〔１－（３,５－二氯苯基）－１－甲基乙基〕－２,３－二氢－６－甲基－５－苯基－４Ｈ－１,３－嗪－４－酮通用名：ｏｘａｚｉｃｌｏｍｅｆ...     

4，4’－硫代双［2－（1，1－二甲基乙基）－5－甲基苯酚］的合成及鉴定

报道了４，４′－硫代双［２－（１，１－二甲基乙基）－５一甲基苯酚］的合成方法及结构鉴定。     

邻二氯苯硝化合成3，4－二氯硝基苯影响因素的考察

邻二氯苯硝化合成３，４－二氯硝基苯影响因素的考察许文松，王庆智（浙江大学化工系，杭州３１００２７）关键词：邻二氯苯，硝化，３，４－二氯硝基苯１前言邻二氯苯（下称Ｏ－ＤＣＢ）硝化的主要产物是３，４－二氯硝基苯（下称３，４－ＤＣＮＢ）。３，４－ＤＣＮＢ经...     

聚甲基四苯基苯硅烷的合成及非线性光学性质的研究

在甲苯中，将甲基四苯基苯二氯硅烷与金属钾反应，或甲基四苯基苯二氯硅烷分别与甲基乙烯基二氯硅烷、甲基苯基二氯硅烷、二甲基二氯硅烷和二苯基二氯硅烷按摩尔比１∶１混合，再与金属钾反应，合成了聚硅烷１、２、３、４和５，分别用元素分析、ＩＲ、ＵＶ、１ＨＮＭＲ和ＧＰＣ作了表征，并测得它们的非线性谐波极化率Ｘ（３）的值分别为８．６×１０－１２、７．９×１０－１２、９．１×１０－１２、６．５×１０－１２和９．３×１０－１２ｅｓｕ。     

1－（3，4，5－三甲氧基苯甲酰基）－4－芳酰基氨基硫脲的合成及其酸催化环化反应的研究

芳酰基异硫氰酸酯与３，４，５－三甲氧基苯甲酰肼在无水乙腈中缩会，制得一系列新的１－（３，４，５－三甲氧基苯甲酰基）－４－芳酰基氨基硫脲。产物的结构已经元素分析、ＩＲ．１ＨＮＭＲ和ＭＳ方法确证。经初步筛选发现一些化合物有抑制大肠杆菌繁殖的活性。     

Zur Strukturaufklärung der Bromierungsprodukte von N-Aryl-2,4-dimethyl-buta-1,3-dien-sultamen-1,4

Structure Elucidation of Bromination Products of N-Aryl-2, 4-dimethyl-buta-1,3-diene-sultames-1, 4 The structure of bromination products of N-aryl-2, 4-dimethyl-buta-1, 3-diene-sultames-1, 4 1a–d , f is determined by 13-C-n.m.r. spectroscopy. As mono bromination product of N-phenylsultam 1a the 4-bromomethyl derivative 2a was isolated. Dibromination of sultames 1 yields 1-brom-4-brommethyl-sultames 3 and by tribromination 1,3-dibrom-4-brommethyl-sultames 4 are obtained.     

Condensation of Unsaturated SCHIFF Bases with ethyl acetoacetate,diethyl malonate and acetylacetone

1, 4-Dihydropyridine derivatives have been obtained by MICHAEL condensation with cinnamylidene anilines 1 or N-p-tolyl-chalcone imine 5 . With ethyl acetoacetate 1 and 5 yield 1-aryl-2-methyl-3-ethoxycarbonyl-4-phenyl-1, 4-dihydropyridines 2 and 6 , with diethyl malonate 1-aryl-3-ethoxycarbonyl-2-oxo-4-phenyl-1, 2, 3, 4-tetrahydropyridines 7 and 8 , and with acetyl acetone 1-aryl-2-methyl-3-acetyl-4-phenyl-1, 4-dihydropyridines 9 and 10 .     

咪唑斯汀的生产工艺改进

首先以4-氟苄基氯和2-氯-1H-苯并咪唑为起始原料合成1-[（4-氟苯基）甲基]-2-氯-1H-苯并咪唑中间体;所得中间体进一步与甲胺哌啶反应得1-[1-（4-氟苄基）甲基-1H-苯并咪唑-2-基]-N-甲基-4-哌啶胺;最后,第二步产物进一步与2-甲硫基-4-嘧啶酮反应制得（2-[[1-[1-（4-氟苄基）-1H-苯并咪唑-2-基]-4-哌啶基]甲胺基]-4（1H）-嘧啶酮）（咪唑斯汀）,总生产收率达54%。     

阿达帕林的合成工艺研究

以1-金刚烷醇、4～溴苯酚为原料,在浓硫酸催化下制得2-（1-金刚烷基）-4-溴苯酚,产物再用硫酸二甲酯甲基化得到2-（1-金刚烷基）-4-溴苯甲醚,2-（1-金刚烷基）～4-溴苯甲醚的格氏化产物再与6-溴-2-萘甲酸甲酯反应,制得6～[3-（1-金刚烷基）-4-甲氧基苯基]-2-萘甲酸甲酯,该产品在氢氧化钠作用下皂化...     

Selective cyclisation of 2, 3, 4, 5-tetra-O-acetyl-galactaric acid bis-[Alkylthio(thiocarbonyl)]hydrazide to Saccharide 1, 3, 4-Oxadiazole,Thiadiazole, and thiadiazoline derivatives

The synthesis of galactaric acid acetate bis[alkylthio(thiocarbonyl)]hydrazide ( 1 , 2 ) is described. Selective cyclisation of both hydrazides 1 and 2 was investigated. Phosphorous oxychloride as cyclising agent led to dehydrative cyclisation and produced 1, 2, 3, 4-tetra-O-acetyl-1, 4-bis(5-S-methyl or — benzyl) 1, 3, 4-thiadiazol-2-yl galactotetritol ( 3 ) or ( 4 ). While thionyl chloride led to dehydrosulfurization and gave 1, 2, 3, 4-tetra-O-acetyl-1, 4-bis(5-S-methyl or -benzyl)-1, 3, 4-oxadiazol-2-yl galactotetritol ( 5 ) or ( 6 ). Finally with triethyl orthoformate as cyclising agent, compounds 1 or 2 , gave 3, 3′-(2, 3, 4, 5-tetra-O-acetyl-galactar-1.6 dioyl)bis[2-ethoxy-2, 3-dihydro-5-S-methyl or benzyl 1, 3, 4-thiadiazole] ( 7 ) or ( 8 ).     

Synthesis of bispiroheterocyclic systems as antimicrobial agents via the reaction of 2-(cycloalkylidene)-1-thia-4-azaspiro[4.4]-nonan-3-one and/or [4.5] decan-3-one with hydrazines,hydroxylamine, urea and thiourea derivatives

1-Oxa-4-thiaspiro[4.4]nonan-2-one ( 1 ) and/or 1-oxa-4-thiaspiro[4.5]-decan-2-one ( 2 ) reacted with 1-naphthylamine to afford 1-thia-4-(1-naphthyl)-4-azaspiro[4.4]nonan-3-one ( 3 ) and/or 1-thia-4-(1-naphthyl)-4-azaspiro[4.5]decan-3-one (4). Reactions of 3 and/or 4 with cyclopentanone or cyclohexanone gave the corresponding 2-cycloalkylidene-4-(1-naphthyl)-1-thia-4-azaspiro[4.4]nonan-3-ones ( 5 and 6 ) and 2-cycloalkylidene-4-(1-napthyl)-1-thia-4-azaspiro[4.5]-decan-3-ones ( 7 and 8 ). Reaction of compounds 5 – 8 with hydrazine hydrate, phenylhydrazine, hydroxylamine hydrochloride, urea and thiourea afforded the corresponding bispirothiazolopyrazolines ( 9 – 16 ), bispirothiazoloisoxazolines ( 17 – 20 ), bispirothiazolopyrimidinones ( 21 – 24 ) and bispirothiazolothiopyrimidinones ( 25 – 28 ) respectively. All the synthesized bispiroheterocyclic derivatives were identified by conventional methods (IR, ¹H-NMR) and elemental analyses. All the prepared compounds were tested for their antimicrobial activities in comparison with tetracycline as a reference compound.     

戊烯-1-炔-4与若干C_5烃和溶剂间汽液平衡数据的测定与关系

用气液色谱法测定了戊烯-1-炔-4(C_5~(?))与异戊二烯(IP)在N-甲基吡咯烷酮(NMP)、二甲基甲酰胺(DMF)和乙腈中的无限稀释下的相对挥发度.结果表明,NMP分离能力最好,DMF次之,乙腈最次,乙腈掺水后可改善分离能力.用鼓泡夹带平衡釜测定了下列体系在0、15、30℃左右的汽液平衡:(1)2-甲基丁烯-2-C_5~(?);(2)正戊烷-C_5~(?);(3)IP-C_5~(?);(4)C_5~(?)乙腈;(5)IP-C_5~(?)-乙腈;(6)IP-C_5~(?)-DMF;(7)IP-C_5~(?)-NMP.用回归出的二元Wilson参数推算体系(5)的三元汽液平衡与实测值比较,汽相组成的平均偏差为0.0114摩尔分数.     

咪唑斯汀的合成新工艺

4-氟苄基氯与2-氯-1H-苯并咪唑反应所得2-氯-1-(4-氟苄基)-1H-苯并咪唑,与4-氯哌啶反应后用甲胺氨解,得1-(4-氟苄基)-2-(4-甲胺基)哌啶基-1H-苯并咪唑,最后与2-甲硫基-1H-嘧啶-4-酮缩合,得H1受体拮抗剂咪唑斯汀,总收率为32%。     

Synthesis,microstructures, and corrosion behaviors of multi-components rare-earth silicates

Multi-components and equimolar rare earth monosilicates, (Y_1/3Dy_1/3Er_1/3)₂SiO₅, (Y_1/3Dy_1/3Lu_1/3)₂SiO₅, (Y_1/4Dy_1/4Ho_1/4Er_1/4)₂SiO₅ and (Yb_1/4Dy_1/4Ho_1/4Er_1/4)₂SiO₅, were prepared by solid-state reactions and the following hot-pressing. Dense microstructures with uniform elemental distributions were obtained for all samples. These investigated multi-components monosilicates exhibit low thermal conductivities and similar coefficients of thermal expansion with SiC. Moreover, they exhibit high corrosion resistances in 1400 °C water vapor, especially, four-components (Y_1/4Dy_1/4Ho_1/4Er_1/4)₂SiO₅ and (Yb_1/4Dy_1/4Ho_1/4Er_1/4)₂SiO₅ experienced almost invariable weights after small weight losses during the initial 0.5 h. All those results indicate that multi-components rare earth monosilicates are promising candidates of environmental barrier coatings for SiC/SiC composites.