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苯乙二醇

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Three ways leads to the synthesis of fenclorin, one way discussed here has 3 steps. Stepl :benzonitrile using as raw material goes though dry hydrogen chloride and becomes a-imino phenylmethyl ether after meet carbinol.

解草啶的合成主要有三条路线,本文选取合成路线是以苯甲腈为原料,经三步反应而成:1、苯甲腈在干燥的氯化氢通入,与甲醇形成亚氨基苯甲醚,通入氨气后置换甲氧基得到苯基脒盐酸盐(收率76.18%)。2、苯基脒盐酸盐在碱性条件下与丙二酸二乙酯环合而得嘧啶醇(收率84.39%)。3、嘧啶醇在三氯氧磷中羟基被氯化得到产品解草啶(收率87.29%)。

A selective and mild PS-DIB/ionic-liquid immobilized 2, 2, 6, 6-tetramethyl-piperidin-4-ol-N-oxyl catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via the iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TeMPO catalyst, 4-(2, 2, 6, 6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from TeMPO and 1, 4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化,制得了负载型二乙酰氧碘苯作为氧化剂。2, 2, 6, 6-四甲基-N-氧自由基哌啶醇与1, 4-二溴丁烷反应生成4-溴丁氧基-2, 2, 6, 6-四甲基-哌啶-1-氧化物,再与N-甲基咪唑发生季铵化反应,生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2, 2, 6, 6-四甲基-N-氧自由基哌啶负载离子液体。

A selective and mild PS-DIB/ionic-liquid immobilized TEMPO catalytic oxidation procedure of alcohols to the corresponding aldehydes and ketones in ionic liquid BF4 at room temperature was developed. The oxidant PS-DIB was prepared via Iodation and acetylation of polystyrene resin. For the preparation of the ionic-liquid immobilized TEMPO catalyst, 4-(2,2,6,6-Tetramethyl-1-oxyl-4-piperidoxyl)butyl bromide was first synthesized from 2,2,6,6-tetramethyl-piperidin-4-ol-N-oxyl and 1,4-dibromobutane.

将聚苯乙烯树脂先碘化再乙酰基化,制得了负载型二乙酰氧碘苯(diacetoxyiodo polystyrene,PS-DIB)作为氧化剂。2,2,6,6-四甲基-N-氧自由基哌啶醇(2,2,6,6-tetramethyl-piperidin-4-ol-N-oxyl,TEMPO)与1,4-二溴丁烷反应生成4-溴丁氧基-2,2,6,6-四甲基-哌啶-1-氧化物,再与N-甲基咪唑发生季铵化反应,生成的溴化季铵盐与四氟硼酸钠进行离子交换制得氟硼酸型2,2,6,6-四甲基-N-氧自由基哌啶负载离子液体TEMPO-IL。

The obtained results show that the primary and secondary alcohols areconverted in good yields, whereas tertiary alcohol and phenol are unreactive.

当原料分别为乙醇、正丁醇、仲丁醇、苯甲醇和苯乙醇时,目标产物碳酸二乙酯、正丁基乙基碳酸酯、仲丁基乙基碳酸酯、苯甲基乙基碳酸酯和苯乙基乙基碳酸酯的产率分别为67.3、52.3、56.7、37.6和32.8%。

The results showed that there were 8 kinds of aliphatic, 5 kinds of esters, 2 kinds of aldehydes, 2 kinds of nitrogen sulfur heterocyclic rings and one kind of hydrocarbon, alcoholics, ketone, lactones respectively in the analyzed 21 kinds of aroma components, and the content of furfural,β-methyl valeric acid, palmitic acid, nicotine, neohytadiene were higher, next were acetyl ethyl propionate, caleric acid, phenyl ethyl acetate, hydroxylic diethyl succinate.

结果表明,在分析出的21种香气成分中,分别有脂肪酸类8种,酯类5种,醛类2种,氮硫杂环类2种,烃类、醇类、酮类、内酯类各l种,其中相对含量较高的物质成分是糠醛、β-甲基戊酸、十六碳酸、烟碱、新植二烯,其次是乙酰丙酸乙酯、异戊酸、苯乙酸乙酯、羟基丁二酸二乙酯等。

The optimal carrier gas velocity of prepared SE-30 series capillary chromatographic columns was studied and used to separate isomeric compounds. The efficiency of SE-30 capillary chromatographic columns has been studied with different diameters, film thicknesses and oven temperatures, using n-do-decane, phenol, aminobenzene, and butyl acetate as test samples.

研究自制的SE-30系列毛细管气相色谱柱的载气最佳线速度,并应用于同分异构体的色谱分离分别用十二烷、苯酚、苯胺、醋酸丁酯作试祥在不同载气线速条件下对不同口径、不同膜厚、不同柱温的SE-30毛细管色谱柱的柱效进行考察,并在最佳线速度条件下分离异戊醇、硝基氯苯、硝基甲苯及二乙苯同分异构体体系。

The process comprises the subsequent steps a through e: a reacting phthalic anhydride with fluorobenzene or a derivative thereof in appropriate reaction conditions; b over reducing the product obtained in step a at the ketone moiety; c reducing the product obtained in step b with sodium dihydro-bis (2- 15 methoxyethoxy) aluminate to the corresponding alcohol ; d chlorinat ing the alcohol obtained in step c ; e inserting CO into the product obtained in step d through an appropriate Pd-containing catalytic system.

该方法包括以下步骤a~e:a使邻苯二甲酸酐与氟苯或者其衍生物在适当的反应条件中反应;b完全还原步骤a中获得的产品的酮部分;c用二氢-二(2-甲氧基乙氧基)铝酸钠将步骤b中获得的产品还原成相应的醇;d对步骤c中获得的醇进行氯化;e通过适当的含Pd的催化剂体系,将CO插入到步骤d中获得的产品中。

We have investigated on the chemical constituents of Nepeta partite collected from Gansu Zhuanglang, and twenty eight compounds were isolated from the methanol extraction of this species by chromatography techniques. Twenty five compounds were identified by means of chemical and spectra methods IR, FABMS, EI-MS,〓, DEPT, and 2D NMR), among which four compounds were new as isopimar-15-en-3β, 8β, 20-triol; phenylethanal-3-O-(2'-glycerin)-5-O-β-D-glucopyranoside; 3-O-linolenoylglyceryl-6'-O-(α-D-galactopyranosyl)-β-D-galactopyranoside; ethyl rosemarinate.

我们对采自甘肃庄浪的康藏荆芥进行了化学成分的研究,利用层析手段从该植物的甲醇浸膏中分离出二十八个化合物,经化学方法和波谱技术(红外,质谱,一维和二维核磁共振谱)鉴定了二十五个化合物的结构,其中四个为新的化合物,它们分别是:异海松-15-烯-3β,8β,20-三醇;苯乙醇-3-O-(2'-甘油基)-5-O-β-D-吡喃葡萄糖甙;3-O-亚麻酰基甘油-6'-0--β-D-吡喃半乳糖甙;迷迭香酸乙酯。

Isopentanol, nitrochlorobenzene, nitrotoluene and diethylbenzene were well separated in the range of optimal carrier gas velocity of 13~17cm/s.

SE-30系列毛细管色谱柱的最佳载气线这范因为13~17cm/s,且在最佳线速度下很好地分离了异戊醇、硝基氯苯、硝基甲苯及二乙苯同分异构体体系。

In this study, new benzo[l,2,3]thiadiazole derivatives were designed according to relationship of structure and efficacy. The 9 novel compounds were synsthesized with following reactions. The chlorine atom in 2-chloro-3,5-dinitro-benzoic acid as beginning raw material was substituted by 2-methylpropane-2-thiol, esterified then with bromoethane, reduced by iron powder and cyclized to obtain ethyl benzo[l,2,3]thiadiazole-7 after diazonation reation.

本论文根据苯并噻二唑诱导剂的构效关系设计了新的苯并噻二唑的结构,并合成了9个未见文献报道的化合物,合成步骤如下:采用2-氯-3,5-二硝基苯甲酸为起始原料,苯环上的氯原子被叔丁基硫醇置换,羧酸由溴乙烷酯化,硝基由铁粉还原,随后经重氮化关环生成苯并[1,2,3]噻二唑-7-羧酸乙酯。

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