Pyridro [2,3-d] pyrimidine 유도체의 합성

姜參龍 명지대학교 1979 明大論文集 Vol.12 No.-

2-(4'-fluoroanilino)-3-pyridinecarboxyamide 〔Ⅰ〕과 ethylcarbonate로 부터 1-(4-fl-uorophenyl) pyrido 〔2,3-d〕pyrimidine-2,4 (1H,3H)-dione 〔Ⅱ〕와 그 유도체 1-(4-fl-uorophenyl)-3-ethylpyrido 〔2,3-d〕pyrimidine-2-4 (1H,3H)-dione(Ⅲ)을 합성하였다. 1. IR 스펙트럼에서 〔Ⅰ〕의 amide가 〔Ⅱ〕와〔Ⅲ〕에서는 보이지 않고, carbonly기, methyl기, methlene기 등이 새로이 보이는 것으로 보아 〔Ⅰ〕이 ethylcarbonate와 축합하여 환화된 것을 알 수 있었다. 2. MS 와 NMR 스펙트럼에서 보여준 분자량과 수소원자의 수는 예상했던 것과 일치하였으며, 원소 분석 결과도 계산 값과 일치하였다. 3. 생성물질〔Ⅲ〕의 녹는 점은 치환기의 종류와 치환된 위치에 따라 규칙적으로 변화되었다. 전자 흡인성이 강한 치환기를 가진 화합물일수록 녹는 점은 낮았으며 p- 치환체는 o-및 m- 치환체보다 녹는 점이 높아지는 경향을 보였다. 1-(4-fluorophenyl) pyrido (2,3-d) pyrimidine-2,4(1H,3H)-dione [Ⅱ] and its derivatives 1-(4-fluorophenyl)-3-ethylpyrido〔2,3-d〕pyrimidine-2,4(1H,3H)-dione〔Ⅲ 〕were synthesized from 2-(4’-fluoroanilino)-3-pyridinecarboxyamide 〔Ⅰ〕 and ethyl-carbonate, 1. The abosorption peak correspond to amide of 〔Ⅰ〕 was not found at 〔Ⅱ〕&〔Ⅲ〕 in the I.R. spectrum, on the other hand, the peaks of carbonyl, methyl, methyl and metyhlene groups were found. Thus it seems to form a ring from condensation of 〔Ⅰ〕and ethylcarbonate. 2. The formula weight and number of hydrogen atoms in M.S. and N.M.R. spectrums were agreement with the expected values, and also the results of elementary analysis were good agreement with calculated values 3. The melthing point of product〔Ⅲ〕depended on the kinds of substituent and the positions that it was substituted, and it was lowered with the strength of elec-tron with drawing character. The melting point of p-substituents showed a tendency to elevate more than those of o-and m-substituents.

松炭油製造 및 林産物 加工에 관한 硏究

姜參龍 명지대학교 1970 明大論文集 Vol.3 No.-

1. The Purpose of this Porject; Even though the wood, especialy pine wood, is abundantty reserved in this country, no attempt of utilization of the manufacturing of pine oil has been presently taken at all. Therefore, there are greatly supplied by import for our developing chemical industry as a raw material So, in this investigation we are aimed at the manufacturing of pine oil from woods and the by product as sawdust, flake etc. ① The pine oil content examined on various kinds of domestic woods. ② The utilization of sawdust, wood flake as a raw material to manufacturing of pine oil. ③ The optimum solvent selection for extraction process. ④ Basic study for scale up. 2. The Content and Scope of this Project; In this investigation, the research project is carried out to study the effects on the pine oil extraction from woods, sawdust, and wood-flake etc. as the raw material investigation. And the more effective process in manufacturing of pine oils with solvent extraction, utilizing domestic woods and the by products. So its applicability with testing the extraction effect and characteristics to various raw material and solvents. 3. The Plan of this Project; This investigation plan of this project is carried out as follows; ① The study of domestic woods and sawdust, wood-flake etc. are considered as the raw material to manufacturing of pine oil. ② The action of various solvents and mixed solvent of extraction of pine oil from woods and the by products (sawdust, flake etc). ③ The optimum condition of pine oil extraction from woods is experimentally determined. ④ The extraction tower size is experimentally determined for the plant basic data. 4. The Experimental Results; In this investigation have been shown the following effects on the pine oil extraction from the woods, sawdust and wood-flake etc. ① From the study on the pine oil contents of various kinds of domestic woods, pine tree, sawdust is a high qualitive and quantive of oleoresin for the raw material in the manufacturing of pine oil. ② The optimum solvents have been found as N-Hexane, Ether, Benzene, And in the view point of industrial plant, the mixed solvents are experimentally determined as Benzene & Alcohol, Ether & Ethyl Alcohol in low cost. ③ The optimum condition in the extraction process have been founded the temperature is the solvent boiling point and the extraction time is 7-8 hour with nontreated sample, and 3-4 hour with pretreated samples. ④ From the experimental result the extraction tower size is excellently worked in solvent extraction, as the L/D Ratio 4-7. 5. The Effect of this Project; ① In this industrial viewpoint; the pine tree, saw dust can be utilized as the raw material in manufacturing of pine oil excellently, considering the content abunduntly reserved in this country. ② On the solvent extraction process in manufacturing of the pine oil, the optimum solvent must be Benzene & Alcohol, Ether & Alcohol for the cost. ③ Extraction tower size have to be the ratio of L/D in 4~7. ④ Not only-saving of the extraction time, but also increasing extraction efficiency, the raw material must be pretreated with soaking in solvent and grinding the size in 14/20 mesh.

氣固系의 熱 및 物質傳達 速度에 관한 硏究

姜參龍,片茂實 명지대학교 1978 明大論文集 Vol.11 No.-

本 硏究는 流噴霧乾燥에 關한 硏究로서 絶對溫度를 측정하여 건조속도와 증발열효율을 구하였고, 또한 噴霧乾燥 操作詩의 열 및 物質傳達關係를 규명하였다. 乾燥機의 軸方向의 길이, 粒子의 初期速度 및 噴霧液體 및 공기간의 질랑유속비를 변수로 해서 수학적인 모델을 설정하여 理論式을 유도하였으며, 특별히 製作된 건구-습구 熱傳對濕度計에 의하여 Local Air Temp., 습도 및 분무입자의 斷熱飽和溫度를 측정하였다. 간단한 이론식으로부터 유도한 축방향의 絶對溫度에 관한 식은 열효율을 생각하여 수면 실험치와 잘 맞았다. 또 열효율과 移動單位數를 聯關시켰으며, 여기서 구한 移動單位數 및 移動單位높이를 이용하여 실제 건조기 설계시 최적치를 얻을 수 있다. 실험결과로는 습도분포를 측정하여 열효율과 乾燥速度와의 相關關係를 규명하였는 바 관계 理論式 과 實驗値가 잘 맞았으며, 또한 丹枉型 流噴霧乾燥機에서는 Plug Flow와 假定하여 設計해도 무방하다는 結論을 얻었다. The heat & mass transfer mechanism was investicated systematically in the view points of spray-dryer design by analyzing the drying rate and thermal efficiency in the cocurrent air spraying dryer. Mathematical model was formulated in terms of the axial distance from the nozzle, drop size, drop velocity, the temperatures of cocurrent air-gas streams, assuming the spray-drying system is an adiabatic process and the rate-determining step is in the side of gas streams. The comparision of experimental results with the theoretical model was brought into such a conclusion that optimum operating condition could be well discussed in the view point of spray-dryer design. The design parameters were correlated in the form of dimensionless groups and NTU method was suggested and appreciated mathematically as a design criteria of air-spraying dryer.

Hexachloroacetone 제조에 관한 연구

姜參龍,李基昌,李光一 명지대학교 1984 明大論文集 Vol.15 No.-

Acetone에 염소화반응을 시켜 Hexachloroacetone을 제조하였다. 이때 촉매의 종류 및 촉매의 양과 반응온도 acetone과 염소와의 주입량등의 요인들을 변화시켜서 최적화 반응조건을 구하였다. 실험결과에 의하면, 지금까지는 Hexachloroacetone을 제조하는 데에는 2단계 과정을 거쳐야 하던지 또는 일단계 과정이라 할지라도 수율이 낮았었으나, 본 실험에서는 촉매를 U.V light와 pyridine을 혼용하므로써 반응시간을 단축시키고 수율을 높일수 있었다. Hexachloroacetone is formed by the reaction of acetone with chlorine. The optimum conditions in this reaction process have been obtained changing the type of catalyst, the main factors, such as the amount of catalyst, reaction temperature and the feeding amount of acetone and chlorine. According to the experimental result reported in the literature two step process has been generally required in forming hexachloroacetone and even one step process has gained the low yield. It was found in this study that the reaction time could be lowered and that the yield may be enhanced using U.V light and pyridine together as a catalyst.