• Title/Summary/Keyword: 고체상 합성

Search Result 78, Processing Time 0.033 seconds

Attempted Synthesis of Carboxin Derivative through Ring Expansion Reaction on Solid Phase (고체상에서 환팽창 반응에 의한 카르복신 유도체의 합성시도)

  • Hahn, Hoh-Gyu;Bae, Su-Yeal;Nam, Kee-Dal
    • The Korean Journal of Pesticide Science
    • /
    • v.9 no.3
    • /
    • pp.185-190
    • /
    • 2005
  • Solid phase synthesis of 16, which is a derivative of the first systemic fungicide, carboxin 1 was described. Reaction of 1,3-oxathiolane derivative with solid resin of 4-hydroxy-3-nitrobenzophenone 6 gave 9 in 82% yield. Oxidation of sulfur in the solid 1,3-oxathiolane 9 by MCPBA followed by a ring expansion reaction under the acid catalyst afforded the corresponding dihydro-1,4-oxathiin derivative 12. Treatment of the solid 1,3-oxathiolane 9 with p-methoxyaniline resulted in 1,3-oxathiolane 14, 1,3-oxathiolane sulfoxide 15, dihydro-1,4-oxathiin 16, and acetoacetanilide derivative 17 in 41%, 35%, 14%, 10% yields, respectively.

A Solid Phase Synthesis of Dihydro-1,4-dioxin and Dihydro-1,4-oxathiin Carboxanilides Using Polymer-bound Oxime Ester (고체상에 연결된 옥심 에스테르를 이용한 다이하이드로-1,4-다이옥신 및 다이하이드로-1,4-옥사티인 카르복스아닐라이드 유도체의 고체상 합성)

  • Hahn, Hoh-Gyu;Bae, Su-Yeal;Nam, Kee-Dal
    • The Korean Journal of Pesticide Science
    • /
    • v.10 no.1
    • /
    • pp.1-6
    • /
    • 2006
  • A methodology for the syntheses of carboxanilides using solid support of 4-chloro-3-nitorbenzophenone oxime resin 5 was developed. Condensation of 4-chloro-3-nitorbenzophenone resin 6 with hydroxylamine hydrochloride salt gave oxime resin 5. The reaction of oxime resin 5 with dioxin and oxathiin derivatives 7a-d afforded the corresponding polymer-bound dioxin and oxathiin derivatives 9a-d. These polymer-bound resins 9a-d were treated respectively with aniline in the presence of acetic acid resulted in the corresponding dioxin carboxanilides 10a-d (yield, 5%-quantitative).

Synthesis of Aminofuroxan Derivatives for the Alkyne Formation on Solid Surface and e-Beam Mediated Fragmentation in Gas Phase (고체상 표면에서 알카인 생성을 위한 아미노퓨록산 유도체의 합성과 전자빔에 의한 기체상 분해반응)

  • Heo, Jeong-Mu;Kim, Gi-Young;Hwang, Kwang-Jin
    • Journal of the Korean Chemical Society
    • /
    • v.51 no.2
    • /
    • pp.160-164
    • /
    • 2007
  • Aminofuroxan derivatives 3 and 4 were prepared by the reaction of chlorofuroxan 2 with butyl and benzyl amines, respectively. E-beam mediated fragmentation of aminofuroxans 3, 4 in mass spectrometer was analyzed in a view of the corresponding alkyne formation.

Study on Effect of gas superficial velocity on particle behavior in three phased Slurry Bubble Column Reactor (3상 Slurry Bubble Column Reactor에서 기체유속에 따른 고체입자의 거동에 대한 연구)

  • Yang, Jung-Hoon;Yang, Jung-Il;Lee, Ho-Tae;Kim, Hak-Joo;Chun, Dong-Hyun;Jung, Heon
    • 한국신재생에너지학회:학술대회논문집
    • /
    • 2009.06a
    • /
    • pp.876-879
    • /
    • 2009
  • Fischer-Tropsch 합성 반응과 같은 slurry bubble column reactor에서는 반응 속도를 증진시키기 위해서는 서로 다른 상간의 접촉 면적을 최대화함으로써 물질 전달을 원활하게 유지하여야 한다. 특히 Fischer-Tropsch 합성 반응에서는 반응물인 기체가 촉매로서 기능하는 고체 표면으로의 external mass transfer가 효과적으로 이루어져야 하기 때문에 반응기 내의 기체의 거동뿐만 아니라 고체인 촉매의 분포에 대한 연구가 활발하게 이루어지고 있다. 따라서 본 연구에서는 반응기 내에 기체의 superficial velocity를 변화시키면서 기체의 hold up 뿐만 아니라 고체 입자의 분포특성에 대하여 관찰하였다. Superficial velocity가 증가함에따라 gas hold up의 경우, 일정하게 증가하다가 6 cm/sec 이상에서 그 증가폭이 감소하였다. 즉 6 cm/sec이상에서 turbulent flow regime을 형성하였다. 또한 고체입자의 분포 역시 기체의 superficial velocity가 증가함에따라 보다 균일하게 되는 것을 확인할 수 있었다.

  • PDF

Optimization of Automated Solid Phase Extraction-based Synthesis of [18F]Fluorocholine (고체상 추출법을 기반으로 한 [18F]Fluorocholine 합성법의 최적화 연구)

  • Jun Young PARK;Jeongmin SON;Won Jun KANG
    • Korean Journal of Clinical Laboratory Science
    • /
    • v.55 no.4
    • /
    • pp.261-268
    • /
    • 2023
  • [18F]Fluorocholine is a radiopharmaceutical used non-invasively in positron emission tomography to diagnose parathyroid adenoma, prostate cancer, and hepatocellular carcinoma by evaluating the choline metabolism. In this study, a radiolabeling method for [18F]fluorocholine was optimized using a solid phase extraction (SPE) cartridge. [18F]Fluorocholine was labeled in two steps using an automated synthesizer. In the first step, dibromomethane was reacted with [18F]KF/K2.2.2/K2CO3 to obtain the intermediate [18F]fluorobromomethane. In the second step, [18F]fluorobromomethane was passed through a Sep-Pak Silica SPE cartridge to remove the impurities and then reacted with N,N-dimethylaminoethanol (DMAE) in a Sep-Pak C18 SPE cartridge to label [18F]fluorocholine. The reaction conditions of [18F]fluorocholine were optimized. The synthesis yield was confirmed according to the number of silica cartridges and DMAE concentration. No statistically significant difference in the synthesis yield of [18F]fluorocholine was observed when using four or three silica cartridges (P>0.05). The labeling yield was 11.5±0.5% (N=4) when DMAE was used as its original solution. On the other hand, when diluted to 10% with dimethyl sulfoxide, the radiochemical yield increased significantly to 30.1±5.2% (N=20). In conclusion, [18F]Fluorocholine for clinical use can be synthesized stably in high yield by applying an optimized synthesis method.

A Review on the Wet Chemical Synthesis of Sulfide Solid Electrolytes for All-Solid-State Li Batteries (전고체전지용 황화물 고체전해질 습식 합성기술 동향)

  • Ha, Yoon-Cheol
    • Journal of the Korean Electrochemical Society
    • /
    • v.25 no.3
    • /
    • pp.95-104
    • /
    • 2022
  • The development of non-flammable all-solid-state batteries (ASSLBs) has become a hot topic due to the known drawbacks of commercial lithium-ion batteries. As the possibility of applying sulfide solid electrolytes (SSEs) for electric vehicle batteries increases, efforts for the low-cost mass-production are actively underway. Until now, most studies have used high-energy mechanical milling, which is easy to control composition and impurities and can reduce the process time. Through this, various SSEs that exceed the Li+ conductivity of liquid electrolytes have been reported, and expectations for the realization of ASSLBs are growing. However, the high-energy mechanical milling method has disadvantages in obtaining the same physical properties when mass-produced, and in controlling the particle size or shape, so that physical properties deteriorate during the full process. On the other hand, wet chemical synthesis technology, which has advantages in mass production and low price, is still in the initial exploration stage. In this technology, SSEs are mainly manufactured through producing a particle-type, solution-type, or mixed-type precursor, but a clear understanding of the reaction mechanism hasn't been made yet. In this review, wet chemical synthesis technologies for SSEs are summarized regarding the reaction mechanism between the raw materials in the solvent.

Determination of thyroid hormones by solid-phase extraction using high performance liquid chromatograph/diode array detector/electro-spray ionization mass spectrometry in urine samples (HPLC/DAD/ESI-MS 및 고체상 추출법을 이용한 뇨시료중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
    • /
    • v.19 no.6
    • /
    • pp.519-528
    • /
    • 2006
  • An analytical method for the determination of thyroid hormones in urine samples has been studied by using solid-phase extraction and high-performance liquid chromatography/diode array detector/electro-spray mass spectrometry. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 100 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile, and UV spectra and mass fragment could be confirmed. The extraction recoveries of thyroid hormones in the urine samples (pH 3) were in the range of 89.0-113.1% with solid-phase extraction by C18, followed by elution with 4 ml of methanol/ammonium hydroxide (9 : 1). The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.992 to 0.998 and the detection limits of all analytes were obtained in the range of 2-4 ng/ml (3.8-13.0 pmol/ml).

A Study on the Preparation of Hollow Microbeads Using Hydroxypropyl Chitosan (키토산 유도체를 이용한 화장품용 중공 마이크로비드의 제조에 관한 연구)

  • 하병조
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.24 no.1
    • /
    • pp.7-24
    • /
    • 1998
  • 게 껍질로부터 얻은 키틴을 탈아세틸화하여 키토산을 얻었으며, 얻어진 키토산의 유기용매에 대한 용해성을 향상시키기 위해 알칼리 조건에서 고압반응ㅇ기를 사용하여 프로필렌옥사이드와 반응시켜 치환율 3.5의 히드록시프로필 키토산을 합성하였다. 합성된 히드록시프로필 키토산은 고체상 CP/MAS 13C-NMR, 1H-NMR, FT-IR을 통해 반응이 키토산의 6번 탄소의 수산기와 2번 탄소의 아민기에 주로 일어났음을 알 수 있었다. 또한 X-선 회절분석을 통해 키토산의 결정성이 프로필렌옥사이드와의 반응에 의해 크게 감소하였음을 알 수 있었고, 그 결과 유기 용매에 대한 용해성이 현저히 증가되는 현상을 나타내었다. 한편, 히드록시프로필 키토산을 수상에 녹인 후 W/O 에멀젼상에 서 알칼리 촉매를 사용항 에피클로로히드린과 가교반응을 실시한 결과 내부가 비어있는 중공 마이크로비드를 얻을 수 있었다. 전자현미경을 통한 분석결과 중공 마이크로비드의 껍질의 내부에는 스킨층이 형성되어 있었으며, 외부 표면은 다공성이 높은 비대칭 막으로 되어 있음을 확인할 수 있었다.

  • PDF

Process variables of gamma-type aluminum trihydride in wet chemical synthesis (감마형 삼수소 알루미늄 습식합성반응의 공정변수 연구)

  • Yang, Yo-Han;Kim, Woo-Ram;Gwon, Yoon-Ja;Park, Mi-Jeong;Kim, Jun-Hyung;Cho, Young-Min
    • Journal of the Korean Applied Science and Technology
    • /
    • v.35 no.1
    • /
    • pp.214-222
    • /
    • 2018
  • Alane(aluminum trihydride, $AlH_3$) is a candidate material involving high energetic capacity for solid propellant or explosives. In this study aluminum trihydride-etherate ($AlH_3{\cdot}(C_2H_5)_2O$) was synthesized through a wet process, and solid alane was extracted by controlled crystallization. Alane crystals were grown during the crystallization step with phase conversion of aluminum trihydride-etherate to alane using an anti-solvent. Stable crystal forms were found by a 2 hour crystallization process at $85^{\circ}C$. Finally the extracted solid aluminium trihydride consisted mainly of ${\gamma}-type$ with $50-100{\mu}m$ in size.

Photo-induced Cationic Polymerization of Vinyl Ethers in the presence of Diphenyliodonium Salts (I) (디페닐요오드늄 염 존재하에서의 비닐 에테르의 광양이온중합 (I))

  • 권순홍;마석일
    • Proceedings of the Korean Fiber Society Conference
    • /
    • 2002.04a
    • /
    • pp.45-48
    • /
    • 2002
  • 양이온 리빙 중합은 분자량 분포가 좁으며 분자량 및 말단기를 조절할 수 있고 블록공중합체의 합성이 용이하다는 장점이 있어 많은 연구들이 진행되어 왔다$^1$. 그러나 액체 또는 기체상의 개시제를 사용함으로 엄격히 건조된 상태의 중합계를 유지하기 위해 많은 주의를 기울여야 하는 단점이 있다. 본 연구실에서는 이러한 단점을 극복하기 위해 고체상인 요오드화 디페닐요오드늄(DPII)와 요오드화 아연을 광양이온 개시계로 이용한 이소부틸비닐에테르(IBVE)의 광양이온 리빙 중합을 보고한 바 있다. (중략)

  • PDF