• 공업화학
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• 제25권3호
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• pp.337-339
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• 2014

본 연구의 내용은 Dimethyl terephthalate의 생성 과정 중 필연적으로 생성되는 부산물인 Methyl 4-formylbenzoate를 이용해 one-pot reaction을 통한 p-Aminobenzoic acid를 얻는 방법이다. 이 방법은 Methyl 4-formylbenzoate에 chlorine gas와 methylene chloride를 이용해 acid chloride를 형성하고 ammonia gas를 통해 amide를 중간체로 가진다. 생성된 amide는 Hofmann degradation을 통해 p-Aminobenzoic acid로 전환된다. 이 방법은 폐기물인 Methyl 4-formylbenzoate를 재활용하여 기존의 p-Aminobenzoic acid를 수율 90%로 합성하였으며 이는 기존의 p-Aminobenzoic acid 생산과정을 대체할 수 있을 것으로 예상된다.

• 한국응용과학기술학회지
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• 제14권2호
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• pp.93-102
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• 1997

Isothiazoline derivatives is widely used to food, medical drug and industrial goods, cosmetics etcs, and it makes to restrain and to sterilize a breeding of microbe as a preservative and a sterilizing agent. It differs with the raw material of paraoxybenzoic acid derivatives or imidazolydinyl urea to be in use at present, on the efficacy and effect, and has various characteristics. This synthesis makes 3,3'-dithiodipropionic chloride to add a thionyl chloride in 3,3'-dithiodipropionic acid, and 3,3'-dithiodipropionic methyl amide makes to synthesize in a reflux reaction the mono methyl amine to 3,3'-dithiodipropionic chloride. And last synthesis becomes to make chlorination-cyclization molecule doing a reflux reaction in the temperature of $90{\sim}100^{\circ}C$ to mix excessively thionyl chloride and ethylene dichloride to 3,3'-dithiodipropionic methyl amide. The last synthesis material has got in the mixture of 5-chloro-2-methyl-4-isothiazoline-3-one and 2-methyl-4-isothiazoline-3-one, and it is so-called isothiazoline derivatives. The purification of isothiazoline derivatives makes to fuse in ethyl acetate, and makes to decolorize and to deodorize in recrystallization. This experiment has been in synthesis and purification of isothiazoline derivatives, and has tried to measure on the antisepsis and sterilization function of microbe according to pH or content change.

• 공업화학
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• 제10권1호
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• pp.135-137
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• 1999

새로운 인돌 유도체인 항염증제를 합성하기 위하여 ${\alpha}$-benzoyl-1-ethyl-1,3,4,9-tetrahydro-8-ethyl-9-(N-benzoyl)pyrano[3,4-b]indole-1-acetic acid methyl ester(10)을 합성하였다. 출발물질은 7-ethylindole과 oxalyl chloride로 하여 4단계로 이루어졌다. 셋째 단계는 borontrifluoride diethyl etherate을 사용하여 66%로 고리화반응을 하였으며, 환원반응과 고리화반응도 효율적으로 단순화하였다. 최종생성물인 ${\alpha}$-benzoyl-1-ethyl-1,3,4,9-tetrahydro-8-ethyl-9-(N-benzoyl)pyrano[3,4-b]indole-1-acetic acid methyl ester는 4단계에서 얻은 methyl 1,8-dimethyl-1,3,4,9-tetrahydropyrano[3,4-b]indole-1-acetate(etodollic acid methyl ester)를 benzoyl chloride와 반응하여 66%의 수율로 얻었다.

• 한국응용과학기술학회지
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• 제31권3호
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• pp.337-344
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• 2014

이 논문은 온도차에 따라 변화되는 이온성 액체와 낮은 밴드갭을 갖는 고분자인 poly(2-heptadecyl-4-vinylthieno[3,4-d]thiazole)(PHVTT) 간의 상호작용 및 고분자의 거동을 조사하였다. 이온성 액체는 methyl imidazolium chloride([MIM]Cl), butyl methyl imidazolium chloride([BMIM]Cl), tri-butyl methyl ammonium methyl sulfate([TBMA][ $MeSO_4$])를 사용하였으며, 21, 28, 32, $37^{\circ}C$로 온도를 변화시키며 상호작용의 변화를 UV-vis spectroscopy, FT-IR spectroscopy, photoluminescence spectroscopy를 통해 확인한 결과 이온성 액체인 [MIM]Cl, [TBMA][$MeSO_4$]와 PHVTT의 상호작용은 점차 약해짐을 확인할 수 있었지만, [BMIM]Cl은 온도 변화에 따른 상호작용의 변화를 보이지 않았다.

• 공업화학
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• 제4권2호
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• pp.300-307
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• 1993

$Na_2S_2O_4$ 수용액과 $CCl_4$-toluene 용액의 2상에서 유기상에 용해하는 tricaprylmethylammonium chloride 상이동 촉매를 사용하여 methyl methacrylate의 라디칼 중합속도를 측정하여, 액-액 불균일계 접촉계면을 통한 라디칼 중합반응기구를 해석하였다. MMA의 중합속도는 수용액상에 존재하는 $Q^+$ 이온의 농도와 ${S_2O_4}^{-2}$ 이온의 농도의 제곱근에 정비례하고 $CCl_4$와 MMA의 농도에 각각 정비례하였다.

• 약학회지
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• 제33권5호
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• pp.280-284
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• 1989

When 2,6-Dimethyl-4-(3'-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-mono methyl ester(3) was reacted with dimethyl methylene ammonium chloride (5a) and $K_2CO_3$ in DMF, 2,6-dimethyl-4-(3'-nitrophenyl)-5-(N,N-dimethylamino)methyl-1,4-dihydropyridine-3-carboxylic acid methyl ester (6a) was obtained in 41% yield. As the same procedure with compound (3) and the other dialkylaminomethylating reagents (5b, c, d, e), 2,6-dimethyl-4-(3'-nitrophenyl)-5-(N,N-diethylamino)methyl-1,4-dihydropyridine-3-carboxylic acid methylester(6b), 2,6-dimethyl-4-(3'-nitrophenyl)-5-(1'-pyrrolidinyl)methyl-1,4-dihydropyridine-3-carboxylic acid methyl ester (6c), 2,6-dimethyl-4-(3'-nitrophenyl)-5-(1'-piperidinyl)methyl-1,4-dihydropyridine-3-carboxylic acid methyl ester (6d) and 2,6-dimethyl-4-(3'-nitrophenyl)-5-(1'-morpholinyl)methyl-1,4-dihydropyridine-3-carboxylic acid methyl ester (6e) were obtained in 28%, 49%, 48% and 18% yield respectively.

• 한국환경보건학회지
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• 제34권2호
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• pp.161-169
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• 2008

This study evaluates the protective effects of Korean garlic juice against the toxicity of methyl mercuric chloride (MMC) in relation to fetal ossification in pregnant Fischer 344 rats. This study has as its basis, both theory and data that neutral amino acids in garlic juice have protective effects against mercury poisoning. Pregnant rats were dosed in various combination with 20 mg MMC/kg body wt. and 0.5 or 1.0 garlic juice/kg body wt. on the 7th day of gestation. Fetuses were extracted from the dams on 20th day of gestation, and the fetal bones were stained and measured. The results obtained are as follows: 1. Fetal body weights, body lengths, and head length were significantly decreased by as much as 23.5%, 21.3%, 15.5% respectively in 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were almost similar to the controls. 2. The ossification centers were significantly decreased by as much as 35.1% in pelvic phalanges, 53.5% in pectoral phalanges, 74.1% in ternebrae, 76.2% in tail in 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were significantly increased by as much as $81.2{\sim}88.7%$ and $94.8{\sim}98.9%$ of controls. 3. The ossified pectoral girdles were significantly decreased by as much as 66.6% in clavicle, and in other areas $74.2{\sim}87.4%$ in the 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were significantly increased by as much as $81.2{\sim}88.7%$ and $94.8{\sim}98.9%$ of the controls. 4. The ossified pelvic girdles were significantly decreased by as much as 57.1% and 56.1% in two ischium, $67.2{\sim}81.7%$ in metacarpals in the 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were significantly increased by as much as $67.0{\sim}85.6%$ and $90.1{\sim}98.7%$ of the controls. 5. The ossified terenebrae were unchanged or significantly decreased; 0.0% in 5th, 54.1% in 1st, 83.9% in 2nd, 75.0% in 3rd, 72.7% in 4th, 79.8% in 6th of 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were significantly increased by as much as $29.5{\sim}55.1%$ and $54.5{\sim}84.0%$ of the controls. 6. The ossified ribs were significantly decreased by as much as $8.3{\sim}18.0%$ in 20 mg/wt kg methyl mercuric chloride groups (p<0.05). But in the garlic treated groups, they were significantly increased by as much as $87.1{\sim}93.5%$ and $96.3{\sim}99.7%$ of the controls. In conclusion, Korean garlic juice significantly protected against the toxicity of MMC in relation to the fetal ossification in pregnant rats.

• Bulletin of the Korean Chemical Society
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• 제32권6호
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• pp.1945-1950
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• 2011

The pyridinolysis of methyl phenyl phosphinic chloride is investigated kinetically in acetonitrile at -20.0 $^{\circ}C$. The Hammett and Br${\o}$nsted plots for substituent X variations in the nucleophiles are biphasic concave downwards with a break point at X = H, and unusual positive ${\rho}_X$ (= 2.94) and negative ${\beta}_X$ (= -0.48) values are obtained for the strongly basic nucleophiles. A stepwise mechanism with a rate-limiting step change from bond breaking for the weakly basic pyridines to bond formation for the strongly basic pyridines is proposed on the basis of biphasic concave downward Hammett and Br${\o}$nsted plots. Unusual positive ${\rho}_X$ and negative ${\beta}_X$ values are rationalized by the isokinetic relationship. The pyridinolyses and anilinolyses of four $R_1R_2$P(=O)Cl-type substrates, dimethyl, diethyl, methyl phenyl, and diphenyl phosphinic chlorides in acetonitrile are compared to obtain systematic information on phosphoryl transfer reaction mechanism. The combination of the two ligands, Me and Ph, shows unexpected kinetic results for both the anilinolysis and pyridinolysis: greatest magnitude of $k_H/k_D$ (= 2.10) involving deuterated anilines $[XC_6H_4NH_2(D_2)]$ for the anilinolysis, and exceptionally fast rate and biphasic concave downward free energy correlation for the pyridinolysis.

• 대한화학회지
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• 제38권5호
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• pp.372-376
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• 1994

Penicillin으로부터 유도된 4-mercaptoazetidin-2-one(2a)은 염기조건에서 불안정하지만 Et3N이나 pyridine 염기하에서 acetyl chloride, methyl chloroformate, ethyl iodoacetate, diethyl azodicarboxylate 등의 친전자체와 반응하여 sulfur에 acetyl, methoxycarbonyl, ethoxycarbonylmethyl, diethoxycarbonylhydrazineo원자단이 부착된 화합물이 된다. 반면 thiol의 methylation은 methyl iodide와의 반응으로 얻을 수 없고 diazomethane을 사용해야 한다. 또한 화합물 2a의 이성질체인 화합물 3a의 반응성도 화합물 2a와 거의 비슷하다.

• 대한화학회지
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• 제55권2호
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• pp.240-242
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• 2011

CuCl과 N-methyl-2-pyrrolidone을 이용하여 5-bromoindole을 halogen - halogen 교환반응을 통하여 5-chloroindole계 화합물을 합성하는 one-pot대량합성방법을 개발하였다.