Asymmetric Synthesis and Crystal Structure of a Bioactive Morpholine Derivative

A novel morpholine derivative was synthesized by Michael addition/internal nucleophilic substitution of 4-（L）-menthyloxy（1R,2S,5R）-butenolide with phenyl-glyalcohol under mild condition, and its structure was determined by X-ray diffraction. The target compound belongs to orthorhombic, space group P212121 with a = 5.7729（7）, b = 11.5032（14）, c = 25.161（3）A, Mr = 319.35, Z = 4, V = 1670.8（4）A^3, Dc = 1.270 g/cm3, μ（MoKα） = 0.094 mm^-1, F（000） = 680, Flack = 0.01（2）, R = 0.0398 and wR = 0.0914.

An ionic 2D inorganic-organic hybrid of tris[((1H-tetrazol-5-yl)methyl)morpholine] dodecatungstophosphate(Ⅴ) pentahydrate:Synthesis X-ray crystal structure and spectroscopic characterizations

A unique ionic hybrid material[C_6H_(12)N_5O]_3[(PO_4)W__(12)O_(36)]·5H_2O has been synthesized from the reaction of((1H-tetrazole-5- yl)methyl)morpholine andα-H_3[(PO_4)W_(12)O_(36)]·21H_2O.It has successfully been characterized by elemental analysis,IR and ~1H NMR spectroscopies,TGA and single-crystal X-ray diffraction method.The title compound is constructed from the three [C_6H_(12)N_5O]^+ cations andα-Keggin[(PO_4)W_(12)O_(36)]^(3-) polyoxoanion.The most remarkable structural feature of this hybrid can...

Synthesis, Crystal Structure and Biological Activities of 2-(4-Fluorophenyl)-2-oxo-1-(1H-1,2,4-triazol-1-yl) ethyl morpholine-4-carbodithioate

The title compound, 2-（ 4-fluorophenyl ） -2-oxo-1-（ 1H-1, 2,4-triazol-1-yl ） ethyl morpholine-4-carbodithioate, was synthesized and its structure was confirmed by means of IR, MS, 1 H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound possesses some biological activities.

Solid-phase Synthesis of-Haloaldehydes from Polymer-supported 4-(Phenylseleno)morpholine

Polystyrene-supported 4-(phenylseleno)morpholine was synthesized and could be used as an efficient ?selenenylating agent for saturated aldehydes. ?Haloaldehydes were prepared by reaction of polystyrene-supported ?selenoaldehydes with bromine or sulfuryl chloride in good yield and high purity.

Studies of Oxide Layers Grown at 260°C on A106 B Carbon Steel in Aqueous Medium with Ethanolamine or Morpholine

The water chemistry of the secondary coolant in the majority of Nuclear Power Plants is controlled by AVT (All Volatile Treatment), wherein volatile amines are used to maintain the alkaline pH required for minimizing the corrosion of structural materials which one of them is Carbon Steel. In this treatment, ammonia, morpholine and ethanolamine are commonly used as conditioning reagents. In this context, experiments were carried out by exposing carbon steel A106 B samples in a simulated secondary coolant in order to study the nature of the oxide films. The tests were performed in a static autoclave at 260°C using two media: I) hydrazine + morpholine and II) hydrazine + ethanolamine during different exposure periods up to ≈1020 h. The oxide film characterization was mainly studied using Scanning Electron Microscopy and X-ray diffraction. A chemical descaling procedure was used to obtain the material weight loss (W) of samples, the adherent and released oxide. The XRD analyses, for all exposures studied, showed that magnetite was the corrosion product formed in the films grown in both media. The material weight loss, after descaling, could be fitted by a law of the type W = ktn, up to 1020 h of exposure tested, resulting in n = 0.42, k = 6.24 for films grown in medium I) and n = 0.39, k = 6.08 for films grown in medium II) respectively (W is in mg/dm2 and t in h). The higher corrosion product release measured in the medium with morpholine could be important in power plant operation.

Tribological Behaviors of S,B-Containing Morpholine Derivatives as Additives in Rapeseed Oil

无灰的二篇小说和非磷 S ， 包含B morpholine 衍生物， MBOC 和 MBOD ，被准备，他们在油菜籽油( RSO )的 tribological 行为用四球的 tester.Thermal 降级被评估测试被进行用穿的 thermo-gravimetric analyzer.The 识别他们的热稳定性钢球的表面被扫描 .The 结果显示了的电子显微镜学( SEM )调查添加剂拥有了高热的稳定性并且好带负担的

NON-ISOTHERMAL KINETICS OF THERMAL DECOMPOSITION OF A NOVEL ANTITUMOR AGENT 4-{5-[3,4-DIMETHYL-5-(3,4,5-TRIMETHOXYPHENYL) THIOPHEN-2-YL ] -2-METHOXYPHENYL} MORPHOLINE

新反肿瘤 agent.4- 的热分解 {5-[3,4-dimethyl-5-(3,4， thoxyphenynthiophen-2-yl ]-methoxyphenyl} 吗被微分扫描热量测定(DSC ) 和在流动的 Thermogravimetry (DTG ) 方法 120 mL/min 的氮气体评估的 Thermogravimetry (TG )/ 衍生物学习。运动参数被基辛格从相应曲线的分析获得“ s 方法， Ozawa ” s 方法和不可分的方法。结果显示明显的活化能和分解反应的 pre 指数的常数是 106,67 kJ/mol 和 10 ^(6.19 )s^(-1), 分别地。

Synthesis and Characterization of Novel Copolymers Based on 3(S)-Methyl-Morpholine-2,5-Dione

A series of novel copolymers were successfully synthesized by ring-opening polymerization(ROP) of 3(S)-methyl-morpholine-2,5-dione(MMD) and 5-methyl-5-benzyloxycarbonyl-1,3-dioxan-2-one(MBC) using stannous octoate as catalyst.The copolymers were characterized by means of 1 H-NMR and FT-IR spectroscopy.Gel permeation chromatography(GPC) test shows that the average-number relative molecular mass and average-weight relative molecular mass slightly increase with the increase of MBC content in feed.The results of differential scanning calorimetry(DSC) demonstrate that the glass transition temperature of copolymers increases with the increase of MBC content in copolymers.The copolymers of MMD and MBC are amorphous copolymers,as indicated by DSC results,while the homopolymer of MMD is semicrystalline.

均匀沉淀法制备Al_(2)O_(3)负载的铜基催化剂及其催化合成吗啉的研究

以尿素为沉淀剂,通过均匀沉淀法制备了Al_(2)O_(3)负载的铜基催化剂。利用XRD、SEM和H_(2)-TPR等手段对催化剂进行表征,并考察活性组分铜镍摩尔比、载体质量分数和尿素摩尔分数对其催化合成吗啉的影响。结果表明,铜镍摩尔比为3∶1、载体质量占催化剂质量的40%、尿素物质的量占金属硝酸盐物质的量的5.25倍时,所制备催化剂具有最高的催化性能。相比于商品催化剂,均匀沉淀法制备的催化剂具有更低的还原温度、更小的平均粒径、疏松的表面结构和优良的稳定性。

察尔汗盐湖卤水中氯化钠浮选剂十二烷基吗啉在氮化碳光催化剂作用下的降解特性

针对察尔汗盐湖氯化钠浮选尾卤中残留的十二烷基吗啉(DMP)难以有效去除的问题,采用多孔状石墨相氮化碳(mpg-C_(3)N_(4))为光催化剂,系统考察盐湖卤水中典型的高浓度无机盐NaCl、KCl和MgCl_(2)等存在条件下对mpg-C_(3)N_(4)光催化降解DMP浮选剂的影响规律与特性。结果表明,卤水中无机盐对降解过程有显著影响,其中高浓度的NaCl对mpg-C_(3)N_(4)的光催化降解特性有促进作用,当NaCl为80 g/L时,DMP的降解速率相对于无NaCl时提升幅度达到20.59%。KCl在低浓度时也能部分促进降解,其中当KCl为25.5 g/L时,DMP的降解速率相对于无KCl时提升幅度为3.71%。但是,体系中存在的MgCl_(2)对mpg-C_(3)N_(4)光催化降解DMP有较大的抑制作用,当MgCl_(2)为65.2 g/L时,DMP的降解速率相对于无MgCl_(2)时抑制率达到44.90%。最后,通过自由基淬灭实验确定光催化降解DMP的主要活性物种为·O-2,其次为·OH。通过对光催化降解前后的产物进行深入对比分析与表征,结果显示经光催化降解后十二烷基吗啉分子中主要基团特征峰几乎完全消失,这表明DMP分子被有效破坏和降解,中间产物及小分子产物大部分也被有效分解矿化。

双模板剂调控SAPO-34对1-丁烯催化裂解的影响

利用水热合成法,通过调控模板剂吗啡啉和四乙基氢氧化铵物质的量比[n(MOR)∶n(TEAOH)]合成出不同SAPO-34分子筛。采用XRD、SEM、NH_(3)-TPD等测试方法对合成样品进行表征,并考察其在1-丁烯催化裂解制丙烯反应中的催化性能。结果表明,双模板剂相比单模板剂制得的SAPO-34分子筛具有不同的酸性和颗粒尺寸,适宜的[n(MOR)∶n(TEAOH)]可以协同SAPO-34分子筛有更弱的酸强度和B酸酸位,从而抑制裂解过程中氢转移反应的发生。当n(MOR)∶n(TEAOH)=2.0∶0.5时可以最大程度的提升丙烯产率和选择性,在1-丁烯催化裂解制丙烯中具有最高的丙烯产率和丙烯选择性,分别为37.03%和45.78%,可以有效应用于1-丁烯催化裂解反应。

以吗啉与环氧乙烷为原料的无催化剂连续快速合成吗啉乙醇工艺研究

针对以吗啉和环氧乙烷为原料合成吗啉乙醇的反应路线收率不高、反应时间长、安全性不好和需使用催化剂的问题,在以SIMM-V2微混合器和不锈钢管组成的微通道反应器中,进行了连续快速制备吗啉乙醇的工艺研究,考察了反应温度、停留时间、体系压力、物料配比和流量等因素对产物收率的影响。结果表明:利用该反应器,在无催化剂条件下和更短的反应时间内可获得与釜式反应器相当的收率;产物收率随着反应温度、停留时间、环氧乙烷配比的增加均呈现先升高再降低趋势,且相互之间会有影响;存在一个较宽泛的反应条件操作窗口,即在给定某一个条件时,可以通过调节其他条件获得相同的产物收率。在典型的反应条件下,如温度为150℃、吗啉与环氧乙烷摩尔比为1∶1.08、停留时间为3 min、总流量为1 mL min、体系压力为2.5 MPa时,吗啉转化率可达99.55%,吗啉乙醇的选择性为97.1%,远高于釜式反应的结果。

离子色谱法测定别嘌醇中吗啉残留

目的 建立了别嘌醇中痕量吗啉测定的离子色谱方法。方法 采用IonPac CS12(250mm×4.0 mm)阳离子色谱柱;以8~40 mmol·L^(-1)甲烷磺酸溶液洗脱;流速为1.0 mL·min^(-1);进样量为500μL;柱温为30℃;抑制器为CERS 300(4 mm);抑制电流为161 mA;外标法定量。结果 该方法下,空白溶液和别嘌醇均不干扰吗啉的检测。吗啉在0.001 487~0.014 87μg·mL^(-1)与峰面积呈现良好的线性关系(r=0.9991),加样回收率(n=3)在89.99%~118.00%,定量限为1.487 ng·mL^(-1)。室温条件下,吗啉对照品溶液和加标样品溶液分别在46.5 h、38 h内稳定性良好。结论 建立的方法灵敏、准确、专属性强、耐用性好,可用于别嘌醇中痕量吗啉的检测。

Studies on the Oxazaborolidine-catalyzed Enantioselective Reduction of 3-Morpholin-4-yl-1-phenyl-1-propanone with Density Functional Theory

Density functional theory (DFT) has been applied to study the enantioselective reduction of 3-morpholin-4-yl-1-phenyl-1-propanone with borane catalyzed by (S)-4-benzyl-5,5- diphenyl-1,3,2-oxazaborolidine at the B3LYP/6-31G* level. All molecular species involved in the four reaction steps have been fully optimized and the structural parameters are provided, and the micro process of reaction was also investigated. The catalyst-alkoxyborane adduct formed in step III exhibits a B-O-B-N tetra-atomic ring. Reaction coordination calculations show that BH3 can react with 3-morpholin-4-yl-1-phenyl-1-propanone spontaneously, resulting in the need of 2 mol BH3 in the reaction.

丹皮酚吗啉杂合物的合成及抗血小板聚集活性

以丹皮酚为起始原料,在碱性条件下丹皮酚的2-位酚羟基与二溴烷烃经Williamson反应得到中间体丹皮酚溴代烷基醚2a~2e,化合物2a~2e与吗啉经N-烷基化反应得到丹皮酚吗啉杂合物3a~3e。目标化合物3a~3e经过核磁共振氢谱(1H NMR)、红外(IR)和高分辨质谱(HRMS)表征。体外抗血小板聚集活性测试结果表明,所得目标化合物3a~3e对二磷酸腺苷(ADP)所诱导的血小板聚集均具有较强的抑制活性,优于阳性对照药阿司匹林。

甲基橙分光光度法测定钾盐浮选药剂十二烷基吗啉的含量

KCl是盐湖矿产资源开发的主要产品,其总量的80%以上采用浮选法生产。十二烷基吗啉是反浮选法生产氯化钾的常用捕收剂,其含量高低会影响钾盐产品的品质和产量。以1,2-二氯乙烷为萃取剂,甲基橙为络合显色剂,采用分光光度法测定十二烷基吗啉的浓度。结果表明,优化的测定条件:测定波长为505 nm,pH=4.0的醋酸-醋酸钠缓冲溶液加入量4.0 mL,浓度为0.05%的甲基橙显色剂加入量2.0 mL,2.0 mol/L盐酸用量为8.0 mL。校准曲线A=0.1245c+0.0039,相关系数R2=0.9981,十二烷基吗啉在0.5~100 mg/L浓度范围内线性关系良好,最低检出限为0.68×10^(-2)mg/L,标准加入法测定钾盐反浮选精钾母液中十二烷基吗啉浓度的平均相对偏差为-1.36%。该方法测量准确度高、灵敏度好、成本较低,可以用于钾盐生产过程中各阶段、各体系中十二烷基吗啉浓度的测定。

积分分离PID算法在吗啉精制控制系统中的应用

针对常规PID控制算法在吗啉精制塔顶温度控制系统中稳定差,受扰后不易稳定等问题,引入积分分离控制算法,基于西门子S7系列PLC,在STEP7编程软件中编制了积分分离PID控制块程序,并应用于吗啉精制塔顶温度控制系统。结果表明:采用积分分离PID算法后,有效降低了系统的超调振荡幅度,提高了控制系统的稳定性,在生产中取得良好效果。

Utilizing morpholine for purely organic room temperature phosphors

In this article,morpholine,a non-conjugated heterocycle,is embedded intoπsystem to construct single-component organic room temperature phosphorescence(RTP)luminogens.The effect of morpholine on intermolecular interaction,crystal packing modes,and RTP performance is investigated systematically.The experimental and theoretical calculation results illustrate the versatility of morpholine in promoting the n-π*transition and intensifying the intermolecular interactions,which not only enhances the generation of triplet excitons,but also suppresses the nonradiative decay of triplet excitons.Impressively,TMPh containing three morpholine units shows an ultralong lifetime of 1.03 s and a visible afterglow up to 10 s.The unique dual delayed emission and long afterglow property allow potential application of morpholine derivatives in data encryption,and the time-dependent color change of afterglow emission is realized after removing the excitation source,providing a high-level data security.This article provides a new perspective for the design of purely organic RTP system without utilization of metal,or even any heavy atoms.