8 research outputs found
コジン ドウテイ ニ カカワル 4ツ ノ コンニチテキ ココロミ
一人の個人を一人の個人と同定すること、即ち個人同定という概念は、古くから伝統的な法医学や古典的な犯罪学の中に育くまれてきた概念である。今日では、個人情報保護法として、個人を定める情報の保護という視点から、社会的に異なった視点から捉えられている。本稿においては、この個人同定の限界を探る自然科学における今日的な試みを紹介する。2つの日本学術振興会科研費を獲得して試行される4つの試みであり、既に一つは成果が上がりはじめている。この個人同定という概念は、人文科学的にみると仏教をはじめとする幾つかの宗教の奥義にある輪廻転生という思想に結びつく要素を孕んでおり、本稿に紹介する最後の研究は自然科学的なものでありながら、その要素に近づきつつあることを興味深く概観している
雙吡啶硫酮的合成改進
以2-巰基吡啶-N-氧化物為原料,30%過氧化氫-尿素加合物為氧化劑合成了雙吡啶硫酮,最佳反應條件是:n(原料):n(氧化劑)=1:1.25,反應溫度45℃,反應時間1.75 h。粗產物用乙醇重結晶,純度為99.6%,收率為91.6%。并用元素分析、紅外光譜和氫核磁共振譜對產物的結構進行了表征。 At the molar ratio of 1:1.25 and the reaction temperature of 45°C, Dipyrithion was obtained through reacting 2-pyridinethiol-N-oxide with 30% hydrogen peroxide-urea adduct for 1.75 h. The yield and purity were 91.6% and 99.6% respectively. The structures were characterized by elementary analysis, IR and 1H NMR
FeCl3/ZnCl2加壓催化酰化制備4-氯二苯甲酮工業化技術
研究了在加壓和FeCl3/ZnCl2催化下,4-氯苯甲酰氯和苯發生Friedel-Crafts反應制備4-氯二苯甲酮的工藝。157.6 g苯、88.2 g 4-氯苯甲酰氯和1.3 g FeCl3/ZnCl2混合于1 L的高壓釜中,在壓力為(0.85~1.1)×106Pa、溫度為175~185℃的條件下反應8 h,經純化處理得到4-氯二甲苯酮93.1 g,摩爾收率為86.2%,w(4-氯二苯甲酮)=99.8%(HPLC)。探討了壓力、催化劑和投料比等對收率的影響。經過一次性投料4-氯苯甲酰氯175 kg的生產型中試驗證,4-氯二苯甲酮摩爾收率為82.7%。 The preparation of 4-chlorobenzophenone by acylation of benzene with 4-chlorobenzoyl chloride in the presence of FeCl3/ZnCl2 catalyst under pressure was studied.157.6 g benzene was mixed with 88.2 g 4-chlorobenzoyl chloride and 1.3 g FeCl3/ZnCl2 in a 1 L autoclave.The mixture reacted for 8 h under(0.85-1.1)×106 Pa and at 175-185 ℃ to give 93.1 g 4-chlorobenzophenone with a yield of 86.2% and a purity of 99.8%(by HPLC).The effects of pressure,catalyst and ratio of raw materials on the yield were also investigated.The experimental results were proved by a productive scale-up test,in which 175 kg 4-chlorobenzoyl chloride was used as raw material to afford 4-chlorobenzophenone in a molar yield of 82.7%
2,2’-(3-硝基-4-氯苯基)次甲基雙(3-羥基-5,5-二甲基-2-環己烯-1-酮)合成與晶體結構
以3-硝基-4-氯苯甲醛和5,5-二甲基-1,3-環己二酮為原料,二甲基甲酰胺為溶劑,不需催化劑合成一種新的氧雜蒽二酮開環衍生物2,2’-(3-硝基-4-氯苯基)次甲基雙(3-羥基-5,5-二甲基-2-環己烯-1-酮)晶體,確定最佳反應條件是:芳醛和脂肪環酮的摩爾投料比為1∶2,反應溫度為80℃,反應時間為1 h;并對其進行熔點、元素分析、紅外光譜、氫核磁共振及X-射線單晶衍射測定。該晶體為單斜晶系,空間群=P21/n,a=1.95777 (13) nm,b=1.22720 (9) nm,c=1.99687 (14) nm,β=107.719 (2) °,V=4.5700 (6) nm3,Z=8,dC=1.302 g/m3,μ=0.205 mm-1,F (000) =1888。 At the molar ratio of 1:1.2 and 80°C, a novel crystal 2, 2'-(3-nitro-4-chlorobenzyl) methylene bis(3-hydroxy-5, 5-dimethyl-2-cyclohexene-1-one), was synthesized through reacting 3-nitro-4-chlorobenzaldehyde with 5, 5-Dimethyl-1, 3-cyclohexanedione using DMF as the solvent for 1 h in the absence of any catalyst. The structure was characterized by melting points, elemental analysis, IR, 1H NMR and X-ray single crystal diffractometer. The result shows the crystal in monoclinic crystal system and P21/n space group. Crystallographic date: a=1.95777(13) nm, b=1.22720(9) nm, c=1.99687(14) nm, β=107.719(2)°, V=4.5700(6) nm3, Z=8, dC=1.302 g/m3, μ=0.205 mm-1, F(000)=1888
合成2-(三溴甲磺酰基)吡啶的工藝改進
聚乙二醇-400催化2-氯吡啶(1)與甲硫醇鈉反應合成了2-甲硫基吡啶(2);2與次溴酸鈉經氧化和溴化反應合成了2-三溴甲磺酰吡啶(3),其結構經1H NMR,IR和元素分析確證。合成2的最佳反應條件為:1 100mmol,甲硫醇鈉0.12 mol,聚乙二醇-400(1.2 mL)為催化劑,于80℃反應4 h,收率98%。合成3的最佳反應條件為:2 95 mmol,n(2)∶n(溴素)=1.00∶6.58,于8℃反應5 h,收率95.1%,純度99.6%。 2-Methylthiopyridine( 2) was obtained by reaction of 2-chloropyridine and sodium methylmercaptide using polyethylene glycol 400 as the phase transfer catalyst. 2-Pyridyl tribromomethyl sulfone( 3) was synthesized by oxdation and bromination reaction of 2. The structures were confirmed by 1 H NMR,IR and elemental analysis. The optimum reaction conditions at 80 ℃ for 4 h of synthesizing 2 were as followes: 1 was 100 mmol,sodium methylmercaptide was 0. 12 mol,and PEG-400( 1. 2mL) was the catalyst,the yield was 98% . The optimum reaction conditions at 8 ℃ for 5 h of synthesizing 3 were as followes: 2 was 95 mmol,n( 2) ∶ n( bromine) = 1. 00 ∶ 6. 58,the yield was 99. 6% and the purity was 95. 1%
一种平喘药中间体1,1-环丙烷二甲醇的制备
以季戊四醇與氫溴酸為原料、硫酸二乙酯-醋酸為催化劑,回流10h合成二溴新戊二醇,收率為91.7%;以二溴新戊二醇與鋅粉為原料、乙醇-水為溶劑合成1.1-環丙烷二甲醇,最佳條件是:n(二溴新戊二醇)∶n(鋅粉)=1∶1.05,反應溫度80℃(微回流),反應時間7h,收率為87.3%,純度為98.7%,并用元素分析、IR和1 H NMR對1.1-環丙烷二甲醇結構進行了表征。Refluxing for 10 h, 2, 2-bis (bromomethyl)-l, 3-propanediol was synthesised at yield of 91.7% from pentaerythritol and bromohydric acid with diethylsulfate and acetic acid as catalysts. Then at the molar ratio of 1 : 1. 05 and 80 °C, 1, 1-bis (hydroxymethyl) cyclopropane was obtained through reacting 2, 2-bis (bromomethyl)-1, 3-propanediol with zinc powder in ethanol-water medium for 7 h. The yield and purity were 87. 3% and 98. 7% respectively. The structures were characterized by elementary analysis, IR and 1H NMR
聚集诱导发光
聚集诱导发光(AIE)是唐本忠院士于2001年提出的一个科学概念,是指一类在溶液中不发光或者发光微弱的分子聚集后发光显著增强的现象。高效固态发光的AIE材料有望从根本上解决有机发光材料面临的聚集导致发光猝灭难题,具有重大的实际应用价值。从分子内旋转受限到分子内运动受限,从聚集诱导发光到聚集体科学,AIE领域已经取得了许多原创性的成果。在本综述中,我们从AIE材料的分类、机理、概念衍生、性能、应用和挑战等方面讨论了AIE领域最近取得的显著进展。希望本综述能激发更多关于分子聚集体的研究,并推动材料、化学和生物医学等学科的进一步交叉融合和更大发展。 Aggregation-induced emission (AIE), conceptually coined by Prof. Ben Zhong Tang in 2001, refers to a unique photophysical phenomenon non- or weakly emissive luminogens in dilute solutions emit intensely upon aggregation. AIE can solve the aggregation-caused quenching problem that traditional fluorophores are suffering from and hold great technological values for practical applications. The past 20 years have witnessed the rapid development of AIE research, from the restriction of intramolecular rotations to restriction of intramolecular motions, and from AIE to aggregate science, and many original results have been achieved. In this review, we summarize the advances in the field of AIE and its related areas. We specifically discuss the recent progress in AIE area, including material classification, mechanism, concept derivation, property, applications, and challenges. It is hoped that this review will inspire more research into the molecular aggregate level and make significant advances in materials, chemistry and biological sciences
