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Bezaldehyde 및 p-Nitrobenzaldehyde와 Butanone의 반응에 관한 연구
鄭悳商 濟州大學校 1982 논문집 Vol.14 No.-
알카리성 縮合反應에서 두 hydroxyketone III과 IV는 순조롭게 가역반응으로 생성되므로 脫水반응은 생성물의 동일성을 결정하는 과정이고, 直銷異性體 I은 ??가 ??보다 더 크기 때문에 생성되는 것이다. 또 강산에서 이들 β-hydroxyketone들은 바르게 脫水된다. 그러므로 이 조건하에서 생성물을 결정하는 과정은 비가역첨가단계이며, II는 k₃가 k₁보다 더 크기때문에 그에 우선하여 생성된다. IV는 산에서 뿐만 아니라 鹽基에서도 III보다 더 빨리 형성되는데, 이것은 IV의 더 빠른 반전(k₄>k₃)이 III과 거의 같은 평형농도를 만들어 주기 때문이다. 이상이 benzaldehyde-butanone 縮合反應에서 觸媒선택성에 관한 本 實驗에서의 結論이라 하겠다. 또 p-Nitrobenzaldehyde-butanone 縮合反應에서는, butanone은 알카리에서 methyl 과 methylene두 위치에서 芳香族 aldehyde와 결합하고, 直銷 benzylidene 화합물의 유일한 생성은 脫水反應 단계에서 큰 비율차이에 의한 결과라는 結論을 얻을 수 있다. The hydroxy ketone intermediates 1-phenylpentan-1-ol-3-one and 3-methy1-4-phenylbutane-4-ol-2-one from the reaction between benzaldehyde and butanone have been perpared by the Schopf method. Treatment of either the straightchain isomer1-phenylpentan-1-ol-3-one or the branched isomer 3-methyl-4-phenylbutane-4-ol-2-one with dilute alkali produced the straight chain unsaturated ketone 1-phenyl-1-penten-3-one. Treatment of 1-phenylpentan-1-ol-3-one and 3-methyl-4-phenybutane4-1-2-one with acid afforded 1-phenyl-1penten-3-one and 3-methyl-4-pheny1-3-buten-2-one, respectively, with no evidence of rearrangement. The reaction between p-nitrobenzaldehyde and butanone in alkali yielded three hydorxy ketones indicating that both methyl and methylene positions were attacked to a comparable extent. These results supports a mechanism for the alkaline condensation in which the dehydration of the intermediate hydroxy ketones is a slow step and thus responsible for the exclusive formation of 1-phenyl-1-penten-3-one. The formation of 3-methyl-4-phenyl-3-buten-2-one in acid results from selectivity at the addition step(2) of the reaction
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Saururus Chinensis의 지방산 및 아미노산의 성분 연구
鄭悳商 제주대학교 1992 논문집 Vol.35 No.-
The fatty acids and amino acids in Saururus chinensis, native to Korea, were isolated and identified by gas chromatograph using glass capillary column and amino acid analyzer. Thirteen fatty acids and seventeen amino acids were identified.
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Aminoaluminum Hydride에 의한 카르복시산 에스테르류의 환원반응
정덕상 濟州大學校 師範大學 科學敎育硏究所 1985 科學敎育 Vol.2 No.-
A method for the preparation of aldehydes from esters of carboxylic acids by use of diaminoaluminum hydrides such as bis (4 - methyl 1 - piperazinyl) aluminum hydride (BMPA) dimorpholionaluminum hydride (DMA) and dipiperidionaluminum hydride (DPA) was described. It was found that BMPA, DMA and DPA reduce esters of carboxylic acids of aldehydes in good yield very smoothly without accompanying alcohols.
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2,6-Dimethylpyridine의 존재하에 一次 및 二次아민類로부터 四次암모늄化合物의 合成에 관한 硏究
鄭悳商 제주대학교 1983 논문집 Vol.15 No.-
一次 및 二次아민類는 直接알킬화方法으로 四次까지 전부 알킬화되었고, 알킬화反應速度에 의하여 측정된 親核性度는 매우 감소되는 것으로 나타나기 때문에 立體障碍를 받는 아민類의 陽性子添加에서 立體障碍가 많은 영향을미치지 않는다는 것을 알 수 있었다. 반응아민類보다 鹽基의 세기가 더 큰 有機鹽基는 알킬화反應에서 發生되는 酸과 結合하는데 쓰여졌고, pKa값이 3.86~5.34인 aniline과 그의 誘導體들은 立體障碍를 받는 鹽基이지만 더 큰 pKa값을 갖는 2,6-dimethylpyridine의 존재하에서 완전히 메틸화됨을 볼 수 있었다. Primary and secondary amines have been exhaustively alkylated to their quaternary stage in a one-step procedure. The observation that protonation of sterically hindered amines is only slightly afftected by steric hindrance, whereas nucleophilicity as measured by the rate of alkylation is considerably decreased, has been synthetically utilized. An organic base of greater base strength than the reactant amines has been employed to bind the acid generated in alkylation reactions. Aniline and aniline derivatives with pKa values of 3.86-5.34 have been completely methylated in the presence of the stronger, but sterically hindered base, 2,6-dimethylpyridine(pKa=6.77). The mild and homogeneous reaction conditions resulted in good yields with minimal laboratory manipulations and effort. As an example of the applicability of the method to amines that possess lable functions, the bisquaternary carbamate, 5-(dimethyl carbamoyloxy)-1,3-phenylenebis(trimethylammonium iodide), has been prepared from 3,5-diaminophenyl dimeth-ylcarbamate in a one-step procedure.
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Lithium Aluminum Hydride 및 그 誘道體들의 還元特性의 比較.Ⅰ : 질소 및 유황화합물과 Aluminum Hydride의 反應
鄭悳商 제주대학교 1986 논문집 Vol.22 No.-
Aluminum hydride, in tetrahydrofuran at 0℃, was used as a selective reducing reagent for amides, nitriles, nitro compunds, other nitrogen compounds, and sulfur compounds. Tertiary amides were rapidly reduced, whereas primary amides were reduced more slowly. Nitriles, phenyl isocyanate, and pyridine N-oxide were reduced rapidly. On the other hand, both aliphatic and aromatic nitro compounds, azobenzene, and azoxybenzene proved to be relatively stable to the reagent. Pyridine reacted at a moderate rate with the uptake of one hydride per mole in 12hrs. Di-n-butyl disulfide was reduced only slowly, but diphenyl disulfide and dimethyl sulfoxide were rapidly reduced. Finally, sulfones, sulfonic acis and cyclohexyl tosylate were stable to the reagent under these conditions. It's properties were compared with those of LAH.LTMA and LTBA and it was shown to be relatively effective in selective reductions.
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GC 및 GC-MS를 이용한 Houttuynia cordata와 Saururus chinensis의 휘발성 성분의 비교
鄭悳商 제주대학교 1991 논문집 Vol.33 No.-
본 연구는 한국에서 자생하는 2종의 삼백초과 식물들의 휘발성 성분을 비교하기 위하여 수행되었으며, 그 결과를 요약하면 다음과 같다. 한국산 삼백초의 휘발성 성분을 처음으로 분리하여 확인한 결과, C??H??인 이성질체 화합물들이 주종을 이루었으며, 약모밀(한국산 및 일본산에서 도)-에서는 검출되지 않았던 benzodioxole 계통 의 Safrole(M.W. : 162)이 확인되었다. The volatile constituents in Sururus chinensis, growing in Korea, were isolated and identified by gas chromatography using glass capillary columns(OV-1, PEG-20M and SE-54) and GC-Mass spectrometry. The volatile constituents of Saururus chinensis were very diffent from those of Houttuynia cordata, that is, the former was mainly composed of sesquiterpenoids, while the latter monoterpenoids.
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Saururus chinensis의 Flavonoid성분 연구
鄭悳商 濟州大學校 基礎科學硏究所 1995 基礎科學硏究 Vol.8 No.1
Four Flavonoids such as isoquercitrin. hyperin, quercitrin and rutin were isolated from the aerial parts of Saururus chinensis growing in Cheju. and identified by the comparision of their TLC. GC, and HPLC chromatogram with those of pure authentic compounds.
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濟州道산 括蔞根으로부터 Trichosanthin의 분리 및 확인
이선주,정덕상 濟州大學校 基礎科學硏究所 1999 基礎科學硏究 Vol.12 No.1
Trichosanthin, a protein from the Korean medical herb Trichosanthes kirillowii, was isolated in two essentially quantitative steps involving Superdex chromatography and HPLC. Final purification of trichosanthin was achieved by reverse-phase HPLC employing a Vydac C4 column(0.46×25cm)
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정덕상,이선주,한성빈,강국철 濟州大學校 基礎科學硏究所 1998 基礎科學硏究 Vol.11 No.2
제주도산 손바닥선이장이 함유하고 있는 생리활성 물질들을 확인하고 검색하려는 시도를 하였다. hexane, acetone, methanol, chloroform과 같은 유기용매를 이용하여 손바닥 선인장에서 물질들을 추출하였고 이들의 항균성을 검색하였다. 그 결과 gram negative인 Escherichia coli와 gram positive인 Staphylococus aures에 대하여 성장을 저해하는 항균성 물질들이 존재함을 밝혔다.
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