• 제목/요약/키워드: glacial acid

검색결과 42건 처리시간 0.027초

Mathematical Planning for Revealing Optimal Synthetic Conditions of Naphthalene Chloromethylation

  • Pak, V.V.;Karimov, R.K.;Shakhidoyatov, Kh.M.;Yun, L.M.;Soh, D.W.
    • 동굴
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    • 제71호
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    • pp.1-4
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    • 2006
  • Chloromethylnaphthalene is a valuable compound for obtaining of the plant growing stimulator - -napthylacetic acid. Chloromethylation of naphthalene by paraformaldehyde in the presence of glacial acetic acid, phosphoric and hydrochloric acids at temperature 80 - 85C and duration - 6 hours the -chloromethylnaphthalene yield was 55-57%. Using Box-Wilson method for mathematical planning of experiment carried out optimization of its synthesis for purpose increasing -chloromethylnaphthalene yield. Preliminary, one - factor experiments were carried out for selecting independence main parameters influencing on the synthesis. A full factor experiment of 23 with extended matrix of planning was used for optimization. Aiming to increase the -chloromethylnaphthalene yield, the obtained mathematical model was used for program of sharp raising on the reply surface. The received optimal conditions for the -chloromethylnaphthalene synthesis were selected as following: molar ratio of naphthalene parapfsormaldehyde of 1 : 2 temperature - 105C duration of the reaction - 3 hours. The yield of -chloromethylnaphthalene under these optimal conditions was 75%.

(${\pm}$)-cis-8-Amino-2,3,4,4a,5,10b-hexahydrothiazolo[4,5-f]indeno [1,2-b][1,4]oxazine의 합성 (Synthesis of (${\pm}$)-cis-8-amino-l-2,3,4,4a,5,10b-hexahydrothiazolo[4,5-f]indeno [1,2-b][1,4]oxazine)

  • 마은숙
    • 약학회지
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    • 제52권6호
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    • pp.488-493
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    • 2008
  • 2-Aminothiazole ring as a bioisoster of catechol in dopamine has provided with good oral availability and lipophilic property. 2-Aminoindan, is a rigid form of dopamine, was evaluated as a dopamine D3 agonist with low neurotoxicity. Dopamine D3 agonist was evaluated as selective for the treatment of Parkinson's disease. In order to develop a novel dopamine D3 agonist, we tried to synthesize the aminothiazoloindenoxazine derivative that is a hybrid structure of aminoindenoxazine and thiazole ring. cis-2-Amino-1-indanol (2) was synthesized from 1,2-indandione-2-oxime by catalytic hydrogenation and it was treated with chloroacetyl chloride and NaH in benzene solution to give (${\pm}$)-cis-4,4a,5,9b-tetrahydroindeno[1,2-b][1,4]oxazin-3(2H)-one (6). Nitration of 6 by the mixed acid gave 8-nitro compound (7) and the carbonyl group of 7 was reduced with $LiAlH_4$ to afford compound (8). 8 was reduced to form (${\pm}$)-cis-8-amino-2,3,4,4a,5,9b-hexahydroindeno[1,2-b][1,4]oxazine (9) and finally it was cyclized with KSCN in glacial acetic acid to yield (${\pm}$)-cis-8-amino-2,3,4,4a,5,10b-hexahydrothiazolo[4,5-f]indeno[1,2-b][1,4]oxazine (10).

Chloromethylation of Naphthalene and Mathematical Planning of Experiment for Revealing Optimal Synthetic Conditions

  • V.V. Pak;R.K. Karimov;Kh.M. Shakhidoyatov;L.M. Yun;Soh, Dea-Wha
    • 한국정보통신학회:학술대회논문집
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    • 한국해양정보통신학회 2004년도 SMICS 2004 International Symposium on Maritime and Communication Sciences
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    • pp.36-37
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    • 2004
  • $\alpha$-Chloromethylnaphthalene is a valuable compound for obtaining of the plant growing stimulator - $\alpha$-napthylacetic acid. Chloromethylation of naphthalene by paraformaldehyde in the presence of glacial acetic acid, phosphoric and hydrochloric acids at temperature 80-85$^{\circ}C$ and duration - 6 hours the $\alpha$-chloromethyl-naphthalene yield was 55-57%. Using Box-Wilson method for mathematical planning of experiment carried out optimization of its synthesis for purpose increasing $\alpha$-chloromethylnaphthalene yield. Preliminary, one - factor experiments were carried out for selecting independence main parameters influencing on the synthesis. A full factor experiment of 2$^3$with extended matrix of planning was used for optimization. Aiming to increase the $\alpha$-chloromethylnaphthalene yield, the obtained mathematical model was used for program of sharp raising on the reply surface. The received optimal conditions for the $\alpha$-chloromethylnaphthalene synthesis were selected as following: molar ratio of naphthalene - parapfsormaldehyde of 1 : 2; temperature -105$^{\circ}C$; duration of the reaction -3 hours. The yield of $\alpha$-chloromethylnaphthalene under these optimal conditions was 75 %.

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New Synthesis of Perhydrotriazolotriazoles Catalyzed by TiCl4 under Ambient Conditions

  • Safari, J.;Gandomi-Ravandi, S.;Ghotbinejad, M.
    • 대한화학회지
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    • 제56권1호
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    • pp.78-81
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    • 2012
  • Aromatic 2,3-diazabuta-1,3-dienes in glacial acetic acid with isothiocyanate in the presence of catalyst $TiCl_4$ at room temperature produced via criss-cross cycloaddition reactions the corresponding perhydro[1,2,4]triazolo[1,2-a][1,2,4] triazole-1,5-dithiones in relatively high yields and short reaction time.

뇌하수체 후엽홀몬에 관한 연구 (I) 후엽홀몬의 조제와 그 역가검정 (Studies on the Posterior Pituitary Hormones I. The Preparation and Assay of the Posterior Pituitary Hormones)

  • 김영은;이상섭;정재형
    • 약학회지
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    • 제6권1호
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    • pp.28-34
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    • 1962
  • Oxytocin and vasopressin were extracted from bovine posterior pituitaries and assayed, in many ways. On the assay of oxytocic active substance, it was found the depression method of blood pressure in a chicken was the easiest one among possible methods. The potency of oxytocin which was extracted with glacial acetic acid was 14.2 I.U./mg. On the assay of vasopressin for pressor activity. A full grown healthy male rat was used. Applying a simple artificial respiratory apparatus, the assay could be carried out successfully. The potency of vasopressin was 13.2 I.U/mg.

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졸-겔법에 의한 강유전체 박막의 제작 (Preperation of PZT ferroelectric thin films by sol-gel processing)

  • 이병수;신태현;조기선;육재호;유도현;김용혁;김성오;지승한;이덕출
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 2001년도 하계학술대회 논문집 C
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    • pp.1414-1416
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    • 2001
  • Crack-free and homogeneous compact and epitaxial lead zirconate titanate(PZT) ferroelectric thin films with perovsikte structure have been prepared by sol-eel method. Tetrabutyl titanate, lead acetate and zirconium nitrate are used as raw materials. Glacial acetic acid is used as a catalyst. Ethylene glycol monoethyl ether is used as a solvent. The annealing temperatures of th thin films are 600~900$^{\circ}C$. The values of the remanent polarization Pr, and the coercive field $E_c$, of the PZT ceramic thin films are 46, 35 ${\mu}C/cm^2$ respectively.

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Quantification of Karanjin Using High Performance Liquid Chromatography in Raw and Detoxified Karanj (Pongamia glabra vent) Seed Cake

  • Prabhu, T.M.;Devakumar, C.;Sastry, V.R.B.;Agrawa, D.K.
    • Asian-Australasian Journal of Animal Sciences
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    • 제15권3호
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    • pp.416-420
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    • 2002
  • Various products of karanj (Pongamia glabra) are utilized for industrial, health and animal agriculture applications in the Indian subcontinent. Despite a rich source of protein (CP, 28-34%), karanj cake was found to be slightly bitter in taste and toxic owing to the presence of flavonoid (Karanjin), restricting its safe inclusion in the livestock diets. Feeding trials with raw cake revealed its poor palatability and adverse performance among different categories of livestock including poultry. The present study was, therefore, aimed to detoxify karanj cake by various physico-chemical methods like solvent extraction, water washing, pressure cooking and alkali and acid treatments. The level of residual karanjin in raw and variously processed cake was quantified using high performance liquid chromatography (HPLC). The raw expeller karanj cake was found to contain about 0.19% of karanjin. Though a non-polar solvent, soxhlet extraction of expeller pressed cake with petroleum ether drastically reduced karanjin content (0.01%). Soaking of cake for 24 h in 1% NaOH (w/w) solution was found to reduce karanjin to a major extent with little further benefit by increasing alkali level. Milder alkalies like lime and fertilizer grade urea reduced the karanjin levels marginally. Similar was the case with mineral acids such as HCl and glacial acetic acid. It was, therefore, concluded that solvent extraction of karanj seeds would be the best method of detoxification as well as for more recovery of oil and karanjin.

QuEChERS 전처리와 LC-MS/MS를 이용한 고추 중 침투성농약 Imidacloprid 및 대사물질 동시분석법 (Analysis of Systemic Pesticide Imidacloprid and Its Metabolites in Pepper using QuEChERS and LC-MS/MS)

  • 서은경;김택겸;홍수명;권혜영;권지형;손경애;김장억;김두호
    • 농약과학회지
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    • 제17권4호
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    • pp.264-270
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    • 2013
  • Imidacloprid는 곤충의 신경 독으로 작용하는 침투성 살충제이며, 과일과 채소에 진딧물 등의 해충 방제에 이용되고 있다. 침투성 농약은 작물체 내부로 흡수 이동되어 다양한 대사산물들이 생성되며 이중 일부 대사산물들은 농산물의 안전성에 문제가 되기도 한다. 따라서 농약과 대사산물의 동시분석법은 작물체 내에서 농약의 동태연구 및 농산물의 안전성을 확인하기 위해 필요하다. 본 연구의 목적은 고추 식물체 내에서 imidacloprid와 그 대사산물 4종, imidacloprid urea, imidacloprid olefin, idmidalcoprid guanidine, 그리고 6-chloronicotininic acid의 QuEChERS 법과 LC-MS/MS 시스템을 사용한 동시 분석법을 개발하고자 하였다. 실험방법은 고추 식물체 시료에 1% glacial acetic acid와 아세토니트릴 첨가한 후 추출하였고 그 추출물을 일정량 분취한 후 PSA와 $C_{18}$을 이용하여 정제하였다. 정제된 추출물은 LC-MS/MS로 분석하였으며, 표준정량곡선은 혼합표준용액(Matrix matched standard)를 제조하여 작성하였다. 표준정량곡선의 상관계수는 0.998 이상이었으며, LOQ도 0.05 mg/kg 이하였다. 0.01, 0.04, 0.1, 0.4 mg/kg 4개 수준으로 회수율시험을 수행하였으며, 그 결과 imidacloprid와 그 대사산물의 회수율은 70~120%이었고, RSD는 20%이하였다. 이러한 결과는 본 시험방법이 고추 식물체에서 imidacloprid 및 그 대사산물을 분석하는데 적합하다는 것을 보여준다.

펄프의 표백(漂白)에 관(關)한 연구(硏究) - 모델리그닌의 합성(合成)과 염소화(鹽素化) 처리(處理) - (Study on Pulp Bleaching - Synthesis of Model Lignin Compounds and their Chlorination)

  • 윤병호;이명구;황병호
    • Journal of the Korean Wood Science and Technology
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    • 제12권2호
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    • pp.27-34
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    • 1984
  • In order to investigate the acidic chlorinated compounds in pulp bleaching spent liquor, the lignin model compounds, coniferyl alcohol(mp $74^{\circ}C$), ${\omega}$-(2-methoxyphenoxy)-acetoguaiacone(mp $93^{\circ}C$) and dehydrodiisoeugenol(mp $133^{\circ}C$), were synthesized and chlorinated by chlorine in glacial acetic acid. From the chlorinated products, the following chlorine-containing aromatic compounds were identified by TLC. In coniferyl alcohol the chlorine-substituted compounds at 4-, 5-and 4,5-position of aromatic nucleus were identified and in ${\beta}$-0-4 type the compounds substituted chlorine for alkyl group and/or hydrogen at land 1,4-position of aromatic nucleus expected to be formed by electrophilic displacement from ${\omega}$-(2-methoxyphenoxy)-acetoguaiacone were not identified but the chlorine-substituted compounds at 4-, 5-, 6- and 5,6-position of aromatic nucleus were identified.

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Synthesis of Novel 6,7,8,9-Tetrahydro-5H-5-hydroxyphenyl-2-benzylidine-3-substituted Hydrazino Thiazolo (2,3-b) Quinazoline as Potent Antinociceptive and Anti-inflammatory Agents

  • Selvam, T. Panneer;Kumar, P. Vijayaraj
    • Bulletin of the Korean Chemical Society
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    • 제31권11호
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    • pp.3265-3271
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    • 2010
  • A series of 6,7,8,9-tetrahydro-5H-5-hydroxyphenyl-2-benzylidine-3-substituted hydrazino thiazolo (2,3-b) quinazolines have been synthesized to meet the structural requirements essential for anti-inflammatory and antinociceptive properties. The synthesized series of heterocycles, 6,7,8,9-tetrahydro-5H-5-hydroxyphenyl-2-benzylidine-3-substituted hydrazino thiazolo (2,3-b) quinazoline by the reaction of 6,7,8,9-tetrahydro-5H-5-hydroxy phenyl thiazolo (2,3-b) quinazolin-3(2H)-one with appropriate hydrazine hydrate and ketones/aldehydes in the presence of anhydrous sodium acetate and glacial acetic acid as presented in Scheme 1. Their antinociceptive activity were evaluated by tailflick technique, anti-inflammatory was evaluated by carrageenan-induced paw edema test and their ulcerogenicity index determined by reported protocol. The compounds exhibited the lowest ulcer index ($0.51{\pm}1.63$, $0.48{\pm}1.28$ and $0.50{\pm}1.53$, respectively. The 6,7,8,9-tetrahydro-5H-5-hydroxy phenylhydroxy-2-benzylidine-3-(N'-3-pentylidenehydrazino) thiazolo (2,3-b) quinazoline and 6,7,8,9-tetrahydro-5H-5-hydroxy phenyl-2-benzylidine-3-(N'-2-pentylidene-hydrazino) thiazolo (2,3-b) quinazoline exhibited the most potent antinociceptive and anti-inflammatory activities.