• Title/Summary/Keyword: 2,2':6'

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Synthesis of 2,6-Diamino-4-Nitrotoluene using Gas Chromatography Monitoring in the Reduction of Trinitrotoulene (Trinitrotoluene의 환원반응에서 가스크로마토그래피 모니터링을 이용한 2,6-diamino-4-nitrotoluene의 합성)

  • Kim, Hyoung-Sug;Yu, Jae Chul;Kim, Ho Gi;Kim, Sae Rom;Choi, Keun Bae;Jung, Won Bok;Seo, Won Jun;Kim, Jin-Seuk
    • Journal of the Korea Institute of Military Science and Technology
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    • v.17 no.2
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    • pp.282-288
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    • 2014
  • In this research, we investigated synthetic method of 2,6-DANT that can be used as a chain extender of urethane/urea and epoxy materials in a demilitarization method via chemical transformations considering environmental, economical aspects and stability of process. We was able to identify through GC monitoring that 2,4-DANT and 2,6-DANT were produced when we inject 'hydrazine monohydrate 3.3 eq. by TNT 1 eq.' with a fine metering pump for 30 minutes and then, reflux for an additional 2 hours. We was able to isolate only 2,6-DANT(99.3% purity and 45.0% yield) from mixture of 2,4-DANT and 2,6-DANT through the separating and refining methods using 2,6-DANT solubility in methanol and crystallinity of 2,6-DANT.

Effects of loading method to Improve Storage Quality under Room Temperature in Onion(Allium cepa. L) (양파 간이 저장시 적재방법이 저장성에 미치는 영향)

  • 이찬중;김희대;정은호;서전규
    • Food Science and Preservation
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    • v.9 no.3
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    • pp.282-286
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    • 2002
  • This study was conducted to improve the storability of onion bulbs by loading method under room temperature and to reduce the rot caused by field open storage. Allium cepa cv. Changnyungdeago, late strain, was used for the test at the storage condition of 1-row-6-stairs, 2-rows-6-stairs, 4-rows-6-stairs, 1-rows-8-stairs, 2-rows-8-stairs, and 4-rows-8-stairs. The results obtained art as follows: The mean temperature was maintained lowly 1.6∼3.2$\^{C}$ in 1-row-6-stairs and 1.3∼2.6$\^{C}$ in 2-rows-6-stairs in contrast to 4-rows-8-stairs and the relative humidity was high when loading rows increased. The rotting rates in 1-row-6-stairs, 2-rows-6-stairs, 4-rows-6-stairs, 1-rows-8-stairs, 2-rows-8-stairs, and 4-rows-8-stairs were 11.4%, 11.6%, 12.4%, 14.6%, 13.9% and 16.6%, respectively, and became higher with increased rows and stairs of loading. Total weight loss of onion bulbs were l2.2%, 12.7%, 13.8%, 15.5%, 15.2% and 18.0% in 1-row-6-stairs, 2-rows-6-stairs, 4-rows-6-stairs, 1-row-8-stairs, 2-rows-8-stairs, and 4-rows-8-stairs, respectively. The rot of onion bulbs was caused mainly by Fusarium sp., Aspergilus sp., Botrytis sp., and bacteria.

Enhanced Detection of Glycans by MALDI-TOF Mass Spectrometry Using a Binary Matrix of 2,5-Dihydroxybenzoic Acid and 2,6-Dihydroxybenzoic Acid

  • Kim, Yunjin;Kim, Taehee;Lee, Jihyeon;Im, Haeju;Kim, Jeongkwon
    • Mass Spectrometry Letters
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    • v.4 no.2
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    • pp.38-40
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    • 2013
  • Glycans released from ovalbumin by PNGase F were analyzed by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry using three different dihydroxybenzoic acid (DHB) matrix systems: 2,5-DHB, 2,6-DHB, and a 2,5-DHB/2,6-DHB binary matrix. Relative to the results obtained with the single-component matrices (2,5-DHB or 2,6-DHB), the 2,5-DHB/2,6-DHB binary matrix boasted lower background noise and higher sensitivity. A total of 16 glycan peaks were observed using the 2,5-DHB/2,6-DHB binary matrix, while only 10 and 9 glycan peaks were observed using the 2,5-DHB and 2,6-DHB matrices, respectively.

The Ir(PPh$_3)_2\;(CO)OClO_3\;and\;Ir(PPh_3)_3N_2Cl$ Mediated Activation of Aldehyde C-H Bonds via Chelate-Assisted Oxidative Addition

  • Ko, Jae-Jung;Joo, Wan-Chul;Kong, Young-Kun
    • Bulletin of the Korean Chemical Society
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    • v.7 no.5
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    • pp.338-341
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    • 1986
  • Hydrocarbon solution of $Ir(PPh_3)_2(CO)OClO_3$ reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to yield ${\bar{Ir(Ph_2PC_6H_4-o-CO)}}\;(PPh_3)_2(CO)(H)ClO_4$(1) and ${\bar{Ir(NC_6H_6NC}}C_6H_5)(PPh_3)_2(CO)(H)ClO_4$(2), respectively. The compound $Ir(PPh_3)_2N_2Cl$ also reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to give ${\bar{Ir(Ph_2PC_6H_4-o-C}}O)(PPh_3)_2(H)Cl(3)$ and $Ir(NC_6H_5NCC_6H_5(PPh_3)_2(H)Cl(4)$, respectively. Compounds 1, 2, 3, and 4 were characterized by infrared, $^1H$ NMR, $^{31}p$ NMR, UV spectra, and conductivity measurements.

Cationic Iridium(I) Complex of Ethyl Cinnamate and Hydrogenation of Unsaturated Esters with Iridium(I)-Perchlorato Complex

  • Yang, Kyung-Joon;Chin, Chong-Shik
    • Bulletin of the Korean Chemical Society
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    • v.7 no.6
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    • pp.466-468
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    • 1986
  • Reaction of $Ir(ClO_4)(CO)(PPh_3)_2$ with trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ produces a new cationic iridium(I) complex, [Ir (trans-$C_6H_5CH$ = $CHCO_2C_2H_5)(CO)(PPh_3)_2]ClO_4$ where trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ seems to be coordinated through the carbonyl oxygen rather than through the $\pi$-system of the olefinic group according to the spectral data. It has been found that Ir$(ClO_4)(CO)(PPh_3)_2$ catalyzes the hydrogenation of $CH_2$ = $CHCO_2C_2H_5$, trans-$CH_3CH$ = $CHCO_2C_2H_5$ and trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ to $CH_3CH_2CO_2C_2H_5$, $CH_3CH_2CH_2CO_2C_2H_5$ and $C_6H_5CH_2CH_2CO_2C_2H_5$, respectively at room temperature under the atmospheric pressure of hydrogen. The relative rates of the hydrogenation of the unsaturated esters are mostly understood in terms of steric reasons.

Molecular Species of Triglycerides in Watermelon Seed Oil (수박씨 기름의 triglyceride 분자종에 관한 연구)

  • Chun, Seok-Jo;Park, Yeung-Ho
    • Korean Journal of Food Science and Technology
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    • v.19 no.4
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    • pp.377-381
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    • 1987
  • From the profiles of triglyceride composition and the fatty acid at ${\beta}-position$ of glycerol, triglyceride molecular species were found to be 26 kinds in watermelon seed oil. The major triglyceride molecular species in watermelon seed oil were $C_{18:1}{\cdot}C_{18:2}{\cdot}C_{18:1}$ OLO; 6.4%, $C_{18:0}{\cdot}C_{18:2}{\cdot}C_{18:2}$ SLL; 7.1%, $C_{18:1}{\cdot}C_{18:2}{\cdot}C_{18:2}$ OLL; 16.6%, $C_{16:0}{\cdot}C_{18:2}{\cdot}C_{18:2}$ PLL; 19.6% and $C_{18:2}{\cdot}C_{18:2}{\cdot}C_{18:2}$ LLL; 27.6%, Triglyceride molecular species of watermelon seed oil characterized that LLL species existed more than 27% of the total triglyceride molecular species.

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Synthesis of N-acyl-α-aminosuccinimides and N-acyl-α-aminoglutarimides (N-아실-α-아미노숙신이미드와 N-아실-α-아미노글루탈이미드의 합성)

  • 정대일;김문주;송현애;김윤영;이용균;박유미;최순규;한정태;박민수
    • Journal of Life Science
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    • v.14 no.1
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    • pp.91-97
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    • 2004
  • As a part of our study on the improvement of anticonvulsant, here we report the synthesis of N-acyl-$\alpha$-aminosuc-cinimides 1 and N-acyl-$\alpha$-aminoglutarimides 2. (R)-Benzoic acid 4-benzyloxycarbonylamino-2-oxo-pyrrolidin-1-ylester 6a, (R)-4-nifro-benzoic acid 4-benzyloxycarbonylamino-2- oxo-pyrrolidin-1-yl ester 6b, (R) -4-nitro-benzoic acid 4-benzyloxycarbonylamino-2-oxo-pyrrolidin-1-yl ester 6c, and (R)-propionic acid 4-benzyloxycarbonylamino-2-oxo-pyrrolidin-1-yl ester 6d were synthesized from (R)-2-benzyloxy carbonylamino-succinic acid 3 as a starting meterial. (R)-(3- Benzyloxycarbonylamino-2,6-dioxo-piperidin-1-yloxy)-acetic acid methyl ester 10a, (R)-(3-benzyloxycarbonylamino-2,6-dioxo-piperidin-1-yloxy)-acetic acid ethy1 ester 10b, an d (R)-2-(3-benzyloxycarbonylamino-2,6- diox o-piperidin-1-yl oxy)-propionic acid methyl ester l0c were synthesized from (R)- 3-carbobenzyloxy-amino-glutarmic acid 7 as a starting meterial. The yield, mp, IR, $^1H-NMR,\; and^{13}C$- NMR spectra of the products 6a, 6b, 6c, 6d, 10a, l0b, l0c are summarized in footnote. The biological studies of these compounds are in progress and will be reported in future.

The [M(cod)(PPh$_3)_2] PF_6$ (M = Rh, Ir; cod = 1,5-cyclooctadiene) Mediated Activiation of Aldehyde C-H Bond

  • Ko, Jae-Jung;Joo, Wan-Chul
    • Bulletin of the Korean Chemical Society
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    • v.8 no.5
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    • pp.372-376
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    • 1987
  • Acetone solution of quinoline-8-carbaldehyde reacts with $[Rh(cod)(PPh_3)_2] PF_6$and $[Ir(cod)(PPh_3)_2] PF_6$ to yield $[Rh(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (1) and $[Ir(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (2), respectively. The compound $[Ir(cod)(PPh_3)_2] PF_6$ also reacts with $Ph_2PC_6H_4-o-CHO$ in the acetone / $H_2O$ mixture to give $[Ir(Ph_2PC_6H_4-o-CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (3). Compounds 1, 2, and 3 were characterized by infrared, $^1H$ NMR, $^{31}P$ NMR spectra and conductivity measurement. The $^1H$ NMR spectra of 1, 2, and 3 support the presence of a terminal hydride that is cis to the phosphine. The IR band of 3 at 2185 $cm^{-1}$, which is assigned to $\nu$(Ir-H), and the hydride cleavage reaction of 3 with $CCl_4$, provide evidence for the Ir-H bond.

Synthesis of New Cyanomethyl-1,3,5-triazine Derivatives (새로운 Cyanomethyl-1,3,5-triazine 유도체들의 합성)

  • Kim, Jung Hwan;Kim, Un Ju
    • Journal of the Korean Chemical Society
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    • v.40 no.11
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    • pp.681-685
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    • 1996
  • New 6-cyanomethyl-1,3,5-triazine derivatives 4 containing amino, n-propylamino, isopropylamino and anilino groups at 2-and 4-position on the 6-cyanomethyl-1,3,5-triazine ring were prepared from 6-chloro-l,3,5-triazine derivatives 2' and 3 with tert-butyl cyanoacetate. The derivatives of 6-chloro-l,3,5-triazine 2' and 3 containing amino, n-propylamino, isopropylamino and anilino groups at 2- and 4-position on the 6-chloro-1,3,5-triazine ring were prepared from 2,4,6-trichloro-1,3,5-triazine as well as 4,6-dichloro-1,3,5-triazine derivatives 2 with amine derivatives.

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The Stereospecific Synthesis of Abscisic Acid

  • Park, Oee-Sook;Lee, W.Y.;Park, J.C.
    • Korean Journal of Pharmacognosy
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    • v.17 no.1
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    • pp.67-72
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    • 1986
  • A stereospecific synthesis of 3-methyl-5-(1-hydroxy-4-oxo-2,6,6-trimethyl-2-cyclohexen-1-yl)-cis, trans-2,4-pentadienoic acid (abscisic acid) from ${\alpha}-ionone$ has been investigated. Ethyl 5-(2,6,6-trimetyl-2-cyclohexen-1-yl)-trans-4-penten-2-ynoate $({\alpha},{\beta}-acetylenic\;ester)$, which was synthesized from alpha-ionone in two steps, was stereospecifically converted in good yield into ethyl 3-methyl-5-(2,6,6-trimethyl-2-cyclohexen-1-yl)-cis, trans-2, 4-pentadienoate $({\alpha}-ionylideneacetate)$ by the conjugate addition of lithium dimethylcuprate at $-78^{\circ}C$. Basic hydrolysis of the ethyl ${\alpha}-ionylideneacetate$ gave an abscisic acid precursor, 3-methyl-5-(2,6,6-trimethyl-2-cyclohexen-1-yl)-cis, trans-2,4-pentadienoic acid, which can be oxidized to yield abscisic acid.

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