N,N-二甲基-1-(2-二苯膦基)二茂铁乙胺的合成

乙酸(1-二茂铁基乙基)酯1与二甲胺反应制备出N,N-二甲基-1-二茂铁乙胺2,收率74%.在正丁基锂/乙醚的反应体系中,化合物2进一步与二苯基氯化磷反应,制备出N,N-二甲基-1-(2-二苯膦基)二茂铁乙胺3,收率18%.化合物3的结构经1H NMR和31P NMR进行了表征,并进一步研究了其合成机理.     

某些4-氨基-1-氮杂-1,3-丁二烯(Ⅱ)新化合物及其3-氯(Ⅲ)和3-溴(Ⅳ)衍生物的合成

用希夫碱(Ⅰ)在无水三氯化铝(AlCl_3)或二异丙胺锂(LDA)与氯化锌乙醚溶液(ZnCl_2·OEt_2)存在下加成于腈类化合物,制备了一些新的4-氨基-1-氮杂-1,3-丁二烯(Ⅱ)。用N-氯琥珀酰亚胺(NCS)和N-溴琥珀酰亚胺(NBS)与带有3-位烯胺氢原子的化合物Ⅱ合成了3-氯(Ⅲ)和3-溴(Ⅳ)衍生物。全部化合物Ⅱ、Ⅲ和Ⅳ都经MS、~1H和~(13)C NMR定性,文中给出了其MS、~1H和~(13)C NMR数据。     

2-羟基-3-氰基-4-三氟甲基-6-氯吡啶的合成与结构鉴定

通过实验首次发现了2,6-二羟基-3-氰基-4-三氟甲基吡啶氯代反应中两个羟基的单氯代产物,在理论上分析了两个羟基的反应活性不同,确定了参与氯代反应的羟基的位置。通过核磁谱图进行了结构鉴定。并经优化反应条件可选择性只生成单氯代目的产物,简化了合成步骤,提高了反应收率。     

1-（6-氯己基）-3-甲基咪唑氯盐离子液体载体的合成

探讨了新型离子液体载体1-（6-氯己基）-3-甲基咪唑氯盐的简便、高产率的合成方法。先以氯取代醇和氮杂环化合物（N-甲基咪唑、吡啶）为原料,采用一步法合成了一系列带有羟基的功能化离子液体中间体,然后选择其中在室温下呈液态且对于空气和水稳定的1-（6-羟己基）-3-甲基咪唑氯盐,与氯化亚砜发生分子内的亲核取代反应,合成了新型离子液体载体1-（6-氯己基）-3-甲基咪唑氯盐。合成的4种中间体及目标产物采用红外光谱和核磁共振谱1H NMR等对其结构进行了表征。     

7-氨基-4,6-二硝基苯并氧化呋咱的合成反应研究

分析和讨论了以3-氯苯胺为原料,经酰化、硝化、叠氮化热解脱氮及水解合成7-氨基-4,6-二硝基苯并氧化呋咱反应的机理及反应条件.此反应收率高,条件温和.     

5α-还原酶特异抑制剂非那甾胺的合成

以3β-羟基孕甾-5-烯-20-酮-3-醋酸酯为起始原料,经溴仿、酯化、氧化、还原、胺化等反应,得中间产物N-叔丁基-3-羰基-4-氮杂-5-雄甾-17β-甲酰胺,再经碘代反应和脱碘反应脱去1、2位氢合成非那甾胺.     

4-氨基吡啶的绿色合成工艺研究

本文报道改进了传统的4-氨基吡啶合成工艺,采用N2O5作为硝化剂,在非酸介质中进行硝化反应,得到N-氧化硝基吡啶,再利用HCOOH/Zn催化转移氢化法,还原得到产品4-氨基吡啶;反应收率较高,是一种清洁高效,相对成本较低的制备4-氨基吡啶的绿色合成方法.     

一种新型1,3-二硫戊环类化合物的合成与表征

以2-硝基乙烯-1,1-二硫醇钾和N,N-二甲基-2,3-二氯-1-丙胺为原料,通过缩合反应合成了一种新型的二硫戊环化合物N,N-二甲基[(E)-(2-硝基亚甲基-1,3-二硫戊环-4-基)]甲胺。利用1H NMR谱确证了其结构的正确性。用乙腈作溶剂进行重结晶,得到其单晶体,通过X-射线衍射仪解析了空间结构。     

N-苯基-2，4-二氯苯胺合成与表征

以苯胺、氯乙酰氯和2,4-二氯苯酚为原料．吡啶为酰化的酸缚剂,碳酸钾为酚的缩合反应催化剂,氢氧化钠为Smiles重排反应的催化剂,在反应物料配比为n（苯胺）：n（氯乙酰氯）：n（吡啶）：n（碳酸钾）：n（氢氧化钠）=1：1．1：1．2：0．9：1．3,重排反应温度105℃．时间10h,通过酰化、缩合、重排、水解四步“一锅烩”的办法合成了N-苯基-2,4-二氯苯胺,收率为60％,产物结构通过IR、NMR和元素分析进行了确认。     

2-(2-烷氧基乙烯基)-6-苯基-5-氯-3(2H)-哒嗪酮化合物的合成

以2-(2-氯乙基)-5-氯-6-苯基-3(2H) -哒嗪酮和相应的醇为原料在温和的反应条件下,经付-克烷基化、闭环、取代、消除、醚化五步反应合成了5种未见文献报道的新的2-(2-烷氧基乙烯基)-6-苯基-5-氯-3(2H) -哒嗪酮化合物,所有化合物均经IR、1H NMR、13C NMR和元素分析对其结构进行了表...     

正交实验法优化酶解法制备杨梅酒工艺

以冷冻杨梅鲜果为原料采用酶解浸提法制作杨梅酒,研究果胶酶和纤维素酶对杨梅酒出酒率的影响。通过单因素实验对影响杨梅酒出酒率的酶种类、酶解温度、酶解时间、酶底物比四因素进行考察,并通过正交实验法优化了杨梅酶解工艺参数。结果表明：确定果胶酶为酶解用酶,酶解法制备杨梅酒酶最佳工艺参数为酶解温度35℃、酶解时间4h,酶底物比2％。在此条件下,杨梅酒出酒率为（79．4±0．19）％,比同法不加果胶酶出酒率增加25．4％,并且过滤时间明显缩短。     

A comparative study of conventional and supercritical fluid extraction methods for the recovery of secondary metabolites from <Emphasis Type="Italic">Syzygium campanulatum</Emphasis> Korth

Syzygium campanulatum Korth is a plant, which is a rich source of secondary metabolites (especially flavanones, chalcone, and triterpenoids). In our present study, three conventional solvent extraction (CSE) techniques and supercritical fluid extraction (SFE) techniques were performed to achieve a maximum recovery of two flavanones, chalcone, and two triterpenoids from S. campanulatum leaves. Furthermore, a Box-Behnken design was constructed for the SFE technique using pressure, temperature, and particle size as independent variables, and yields of crude extract, individual and total secondary metabolites as the dependent variables. In the CSE procedure, twenty extracts were produced using ten different solvents and three techniques (maceration, soxhletion, and reflux). An enriched extract of five secondary metabolites was collected using n-hexane:methanol (1:1) soxhletion. Using food-grade ethanol as a modifier, the SFE methods produced a higher recovery (25.5%?84.9%) of selected secondary metabolites as compared to the CSE techniques (0.92%?66.00%).     

两个新型三β-二酮化合物的设计、合成和晶体结构

成功合成了两个新型的三苯胺衍生物:三-[4-(4-三氟甲基-1,3-丁二酮)苯基]胺(L1)、三-[4-(4-苯基-1,3-丁二酮)苯基]胺(L2),并使用元素分析、红外、核磁和质谱进行了表征,通过单晶X-射线衍射分析,发现分子具有D-(π-A)3的结构。     

A COMPARISON OF THREE METHODS FOR ESTABLISHING MINIMUM STANDARDS ON THE NATIONAL TEACHER EXAMINATIONS

Minimum standards were established for the National Teacher Examinations (NTE) area examinations in mathematics and in elementary education by independent panels of teacher educators who had been instructed in the use of either the Angoff, Nedelsky, or Jaeger procedures. Of these three procedures, only the Jaeger method requires that normative data be provided to the judges when evaluating the items. However, it was of interest to study the effect such information would have upon the standards obtained using the other two methods. Therefore, the design incorporated three sequential review sessions with the level of normative information different for each. A three-factor ANOVA revealed significant main effects for methods and sessions but not for subject area. None of the interactions was significant. The anticipated failure rates, the psychometric characteristics of the ratings, and other factors suggest that the Angoff procedure, as modified during the second session of this study, yields the most defensible standards for the NTE area examinations.     

Establishing a portfolio assessment framework for pre-service teachers: a multiple perspectives approach

In the field of initial teacher training, portfolios are widely used to assess pre-service teachers' performance as well as the outcomes of university-based teacher preparation programmes. However, little is known about the explicit design of portfolio assessment mechanisms in teacher preparation programmes. Issues related to the design and validation of portfolios for pre-service teacher assessment are a critical area of inquiry for the field of initial teacher training. In this study, perspectives were elicited from school trainee teachers and faculty from a secondary teacher preparation programme to examine the relationships identified among core competencies of a portfolio assessment framework and pre-service candidate learning outcomes. Comparative findings are presented about the relationships identified by the trainee teachers and faculty across the secondary education programme's portfolio core competencies and trainee learning outcomes. A discussion of the findings is presented with implications and future directions highlighted.     

项目教学法在中职校本教材建设中的应用

以建构主义理念为指导,按照发展性原则,围绕"服务学生,就业导向,培养能力"的核心理念,将项目教学法应用到中职校本教材建设中,既能发挥教师的主导作用,又能充分体现学生的主体地位。项目校本教材的编写,应遵循科学性与思想性、规范性与程序性、灵活性与务实性、适度超前与效益最佳等原则,并采用PDCA方法,提高编写质量和使用中的满意度。     

An Ecological Momentary Assessment of Burnout,Rejuvenation Strategies,Job Satisfaction,and Quitting Intentions in Childcare Teachers

Guided by affective events theory, the purpose of this study was to examine the temporal aspects of childcare teacher burnout, particularly as to how feelings of exhaustion throughout the day relate to perceptions of end-of-day job satisfaction and quitting intentions. A secondary purpose of the study was to explore the frequency and type of rejuvenation strategies childcare teachers use to relieve perceived stress throughout the day. Ecological momentary assessment procedures were employed for 1 week to assess exhaustion levels (3 times/day), frequencies and types of rejuvenation strategies (3 times/day), and end-of-day job satisfaction perceptions and quitting intentions (1 time/day) among 50 childcare teachers. Results indicated that childcare teachers’ quitting intentions were positively predicted by emotional exhaustion (β?=?0.52) and negatively predicted by overall job satisfaction (β?=??0.28). Short (≤15 min), infrequently used (one to two times/day) physical or cognitive health reprieve strategies were reported by 86?% of teachers as the most effective for reducing daily stress. Findings suggest that daily accounts of burnout and quitting intentions have both exhaustive and restorative properties.     

Guidance and counseling program development in Botswana

In this article the procedures utilized in developing recommendations for guidance and counseling programming in Botswana are discussed. Initially, the status of guidance and counseling was determined through numerous interviews with individuals in many locations in the country. In addition to the information gained from these interviews, a needs assessment was conducted through reviewing national documents and surveying primary and secondary teachers and secondary students. Questionnaires administered to 106 primary school teachers, 89 secondary school teachers and 405 secondary school students were analyzed.Data from these sources comprised the foundation for recommendations for a sequence of developmental tasks for Guidance and Counseling Program Development in the Botswana Educational System. Six primary counselor roles including 1) Counseling Service, 2) Consulting Service, 3) Information Service, 4) Referral Service, 5) Placement and Follow-up Service and 6) Evaluation and Research Service serve as the basis for these recommendations.     

β-胺基乙基膦酸的合成

报道了一种合成β-胺基乙基膦酸的新方法.以三乙胺为碘化氢的束缚剂,胺与β-碘代乙基膦酸酯作用,得到β-胺基乙基膦酸酯,然后水解得到标题产物β-胺基乙基膦酸.产物经红外光谱、质谱分析确认与文献完全一致.该制备方法,反应条件温和,产率高达83%,显著高于文献值.     

脂肪胺、醛、醇、酸、醚气相碱性与分子结构之间定量关系的拓扑化学研究

根据化学热力学原理和量子力学原理,用拓扑方法探讨了脂肪胺、醛、醇、酸、醚的气相碱性与其分子结构之间的定量关系,发现气相碱性的大小主要取决于分子中亲合基团的特性和烷基基团的种类、数目和烷基基团与亲合基团之间的距离,据此提出了一种能够合理表征脂肪胺、醛、醇、酸、醚的气相碱性(PA)与分子结构之间的定量关系式 PA=251.1886[PA(G)+∑∑B_i(4-v_j)n_j~(i)]~(1/5)式中 PA(G)是与亲合基因特性有关的常数,n_j~(i)(i,j=1,2,3,4)为i级烷基基因j的数目,v_j为烷基基因j的顶点度,B_1=17.4546,B_2=17.5552,B_3=10.5896,B_4=5.5842,PA(-NH_2)=530.84,PA(-NH-)=576.14,PA(-N<)=592.79,PA(-O-)=224.27,PA(-OH)=207.11,PA(-COOH)=263.90,PA(-CHO)=242.11,PA(-HCOO)=280.04.对73种化合物气相碱性的计算结果表明,计算值与实验值的一致性令人满意,平均误差0.335％.