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2-Chloro-2',6'-diethyl-N-butoxymethylacetanilide 의 합성에 관한 연구
우제완,박용성,황영애 상명대학교 자연과학연구소 2000 自然科學硏究 Vol.7 No.-
Chloroacetanilide계 제초제인 butachlor (2-Chloro-2’,6’-diethyl-N-butoxymethylacetanilide)의 Lab. 합성 공정을 최적화하였다 . 2,6-Diethylaniline을 출발 물질로 하여, chloroacetylation, alkylation 반응을 수행하는 2 step process중 정제하지 않고 고순도의 butachlor를 합성하는 공정을 개발하였다. 즉, 2,6-diethylaniline과 chloroacetyl chloride를 dichloroethane 용매하에서 반응시켜 수율 93.70%, G/C정성순도 99.18%의 중간체 2-chloro(2’,6’-diethyl)acetanilide를 얻고, 이를 50% 가성소다와 toluene 용매하에서 butyl chloromethyl ether와 2-phase reaction을 시켜 수율 94.06%, 순도 94.51%의 butachlor를 얻었다. 또한, 개발된 process의 최적 합성 조건에 대한 반복실험을 수행하여 재현성을 확보하였다. Synthetic process of butachlor (2-chloro-2’,6’-diethyl-N-butoxymethylacetanilide) which is one of the chloroacetanilide herbicide was investigated for the optimization of the commercial process. Butachlor was synthesized in two steps reaction ? chloroacetylation and N-alkylation, starting from 2’,6’-diethylaniline to 2-chloro-2’,6’-diethyl-N-butoxymethylacetanilide. The reproducibility for the optimal condition was confirmed by repeating experiments and butachlor was prepared by using this process with 88% yield and 94.5% purity without further purification.
2,3- Dicyano -1,4- Dithiaanthraquinone 의 새로운 제조방법
우제완,이상필,백충훈,이유석 한국공업화학회 1998 응용화학 Vol.2 No.1
Dithianon, 2,3-dicyano-1,4-dithiaanthraquinone, is nonchlorinated quinone derivative. It may be prepared by the reaction of DDM, obtained from CS₂ and NaCN , with 1.4-Naphthoquinone or Dichlon in 3step. We studied on 2 step reaction and optimized for scale-up using Experimental design method.
N - Methyleneamine 의 합성 및 이를 이용한 Chloroacetanilide 계 제초제 합성
우제완,이상필,백충훈,이유석 한국공업화학회 1997 응용화학 Vol.1 No.2
N-mehtyleneamine, which is used as important key intemediate in organic synthesis, coude be generated from the reaction of Amine and 35% Formaline in presence of the inorganic drying agents. The reaction proceeded via equilibrium shift reaction between amine and N-methyleneamine. We could synthesize two kind of Chloroacetanilides herbicides in high yield via 3-step 1-pot reaction using N-methyleneamine as key intermidiate.
살균제 Propineb 의 현수성과 수화성에 대한 계면활성제의 영향
우제완,이상필,백충훈,이유석 한국공업화학회 1997 응용화학 Vol.1 No.2
Serveral surfactants were used during experiments in order to select a wetting and a dispersing agent for a wettable powder (WP) of fungicide Propineb. The content effects of the selected surfactants on the suspensibility and the wettability of wettable powder were investigated. The optimal contents of AES as wetting agent and APS as dispersing agent for a Propineb WP were 3.1 ∼ 4.0% and 4.0 ∼ 5.0 %, respectively.