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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1732885생성일: 2026년 10월 26일

Sodium hydride → 1-(4-chlorophenoxy)-3,3-dimethyl-2-(N-methyl-N-trichloromethylmercapto-carbamoyloxy)-1-(1,2,4-triazol-1-yl)-butane

https://huagongshe.com/reaction/1732885

반응식

참여 물질

역할이름HCID투입량
반응물Sodium hydrideHCID 24758—
반응물TriadimenolHCID 41368—
반응물SodiumHCID 5360545—
반응물Methyl[(trichloromethyl)sulfanyl]carbamyl fluorideHCID 12836648—
용매TetrahydrofuranHCID 8028—
생성물1-(4-chlorophenoxy)-3,3-dimethyl-2-(N-methyl-N-trichloromethylmercapto-carbamoyloxy)-1-(1,2,4-triazol-1-yl)-butaneHCID 8673739038.5%

반응 단계

22.3 g (0.075 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol, in the form of the pure diastereomer, were dissolved in 200 ml of tetrahydrofuran and the solution was added dropwise to 2.3 g of 80% pure sodium hydride in 150 ml of tetrahydrofuran at room temperature, while stirring. Thereafter, the mixture was stirred at 50° C. for 12 hours. After cooling, 17 g (0.075 mol) of N-methyl-N-trichloromethylmercaptocarbamoyl fluoride were added dropwise, at room temperature, to the sodium salt thus obtained, whereupon the temperature rose to about 35° C. The mixture was then heated under reflux for 16 hours, left to cool and concentrated by distilling off the solvent. The oily residue was taken up in 500 ml of methylene chloride, washed twice with 1,000 ml of water each time, dried over sodium sulphate and concentrated. The oil which remained was taken up in 300 ml of isopropyl ether, whereupon it crystallized out. 14.5 g (37% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-2-(N-methyl-N-trichloromethylmercapto-carbamoyloxy)-1-(1,2,4-triazol-1-yl)-butane were obtained in the form of the pure diastereomer of melting point 110°-112° C.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US04239766
출처 데이터셋uspto-grants-1980_12
ORD IDord-010e7313fce5450e928430ebe46a8d9c
출처 메모uspto-grants-1980_12