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hydroxy-2-acetonaphthene was obtained by the hydrolysis of 6-methoxy- 2-acetonaphthene in the presence of HCl (36%) and triethylamine as a catalyst.

摘 要:采用6 甲氧基 2 乙酰萘与浓盐酸在缚酸剂三乙胺存在的条件下进行水解反应制得6 羟基 2 乙酰萘。

The crystal belongs to monoiclinic with space group P2 1/n, a=1.7073(7)nm, b=1.7447(7)nm, c=2.4333(10)nm,β=109.694(7)°, Z=4,V=6.824(5)nm 3, D x=1.282g/cm 3,μ=0.793mm -1, F(000)=2696, R 1=0.0563, WR 2=0.1539. In the crystals of compound, the tin atoms rendered seven-coordinate in a distorted pengonal bipyramidal structure.

我们以 NEt3 作缚酸剂,用 Ph3 Sn Cl与 2 ,6 -吡啶二甲酸以 1∶ 1摩尔比反应时,没有得到预期产物 Ph3 Sn O2 C(2 ,6 - Py)CO2 H ,而是得到一种 Sn- Ph键断裂的离子型有机锡化合物(Scheme1 )。

Synthesis of Antidote of N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane BI Hong-mei, ZHANG Jin-yan, LIANG Ying, SHEN Yong (College of Arts and Sciences Heilongjiang August First Reclamation University, Daqing 163319, Heilongjiang, China) Abstract: N-Dichloroacetyl-2-methyl-1-oxa-4-aza-spiro-4.4-nonane was synthesized by one pot method with isopropanolamine, cyclopentanone and dichloroacetyl chloride. The optimum reaction conditions obtained are as follows:the proportion in moles of the above materials is 1∶1∶1.2, reaction solvent is toluene, reaction temperature is -15 to -10 ℃,reaction time is 3 h, under the optimum condition, the yield of the compound is 50.0%.

除草剂解毒剂N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷的合成毕洪梅,张金艳,梁英,沈勇(黑龙江八一农垦大学文理学院,黑龙江大庆 163319)摘要:以33%的氢氧化钠水溶液为缚酸剂,异丙醇胺、环戊酮和二氯乙酰氯为原料,采用&一锅法&合成了N-二氯乙酰基-2-甲基-1-氧杂-4-氮杂-螺[4.4]壬烷,采用正交实验法得到最佳反应条件:反应原料摩尔比为1∶1∶1.2,苯作溶剂,反应的温度为-15 ℃~-10 ℃,搅拌时间为3 h,产率达到50.0%。

Trifluoromethyl-3-heptadfluoroisopropyl-2-perfluoropentene-4-(N',N'-dimethylamino propyl) imino was prepared by the reaction of hexafluoropropene timer with N,N-dimethyl propanediamine in the molar ratio 1:1.0 at room temperature for 8h, and the structures of VIII were identified by IR and NMR spectra.

以六氟丙烯三聚体与N,N-二甲基丙二胺为原料合成叔胺2-三氟甲基-3-七氟异丙基-2-全氟戊烯-4-(N',N'-二甲胺丙基)亚胺,利用红外光谱和核磁共振确定其结构,并通过对合成条件的考察得其最佳合成条件:乙醚为溶剂,碳酸钠为缚酸剂,摩尔投料比为1:1.0,在室温下反应8小时。

Then sodium ethoxide was used as base,the nucleophilic substitution of 2-pyrrolidone with the intermediate provided nefiracetam.

以碳酸钠为缚酸剂,摩尔比为1︰1的2,6-二甲基苯胺与氯乙酰氯反应合成了中间体2-氯-N-(2,6-二甲基苯基)乙酰胺;在强碱乙醇钠作用下,2-吡咯烷酮再与2-氯-N-(2,6-二甲基苯基)乙酰胺经亲核取代合成了目标化合物奈非西坦。

Fourteen new pyrethroids containing isoxazole were designed and synthesized from 4-isopropyl-3-substituted phenyl-5-hydroxyl isoxazoles as major material, whose structures were also characterized by IR, 1H NMR and elemental analysis.

以4-异丙基-3-取代苯基-5-羟基异噁唑和3-苯氧基苄基溴为原料,三乙胺为缚酸剂,设计并合成了14个未见报道的4-异丙基-3-取代苯基-5-异噁唑基-(3'-苯氧基)苄基醚。通过红外光谱、核磁共振、元素分析等手段,确证了它们的化学结构。

To improve the yield of an Amide-type Tripodal Ligand and investigate its coordination with rare earth ion under mild condition,a series of Amide-type Tripodal Ligands(L1—L4) have been prepared by the reactions of nitrilotriacetic acid and oxalyl chloride with four kinds of amides,respectively.

为了提高酰胺型三脚架型配体的产率,进一步研究其与稀土离子的配位形式及配合物的荧光性能,以氨三乙酸为母体,草酰氯为氯化试剂,与4种胺在较温和的条件下合成了具有三脚架型结构的配体(L1—L4),并考察了实验条件、反应温度、反应体系溶剂、缚酸剂、反应时间及催化剂对反应产率的影响。

Kinetic spectrophotometric method for the determinationof trace nitrilotriacetic acid;2. To improve the yield of an Amide-type Tripodal Ligand and investigate its coordination with rare earth ion under mild condition,a series of Amide-type Tripodal Ligands(L1—L4) have been prepared by the reactions of nitrilotriacetic acid and oxalyl chloride with four kinds of amides,respectively.

为了提高酰胺型三脚架型配体的产率,进一步研究其与稀土离子的配位形式及配合物的荧光性能,以氨三乙酸为母体,草酰氯为氯化试剂,与4种胺在较温和的条件下合成了具有三脚架型结构的配体(L1—L4),并考察了实验条件、反应温度、反应体系溶剂、缚酸剂、反应时间及催化剂对反应产率的影响。

The thermal property studies indicate that the mass loss of compound B was 54.39% at 242.2~750℃, and when the temperature was 1000℃, there was 25.11% char residue left, which showed that the title compound has a good thermal stability and char forming capability. Using acetonitrile as the solvent instead of trichloromethane or 1, 2-dichloethane gave higher yield. During the synthesis, the yield was very low when triethylamine was used as acid acceptor alone, and when a little amount of 4-dimethylaminopyridine was added at the same time, the yield could be 81%.

结果表明,所合成的化合物B的结构与预期的结构一致;热性能研究表明,化合物B在242.2~750℃质量损失为54.39%,1000℃时仍有25.11%的炭残渣,显示出优异的热稳定性和成炭性;在相同反应条件下,用乙腈作为溶剂的反应产率比使用氯仿和二氯乙烷为溶剂的高,并且在合成过程中,单独使用三乙胺作为缚酸剂时产率很低,而当同时加入少量4-二甲氨基吡啶时,产率可达81%。

And the best conditions were as following: alcohol as solvent, sodium carbonate as acid absorbing agent, refluxing for 8h.

通过因素分析确定了合成RNB的最优化条件为:以乙醇为溶剂,Na_2CO_3为缚酸剂回流反应8h。

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