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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 37589생성일: 2026년 10월 24일

Toluene → (E)-2-cyano-3-(2,2-difluoro-1,3-benzodioxol-4-yl)-2-propenoic acid ethyl ester

https://huagongshe.com/ko/reaction/37589

반응식

참여 물질

역할이름HCID투입량
반응물TolueneHCID 1140—
반응물N,N,N',N'-TetramethylethylenediamineHCID 8037—
반응물2,2-Difluoro-1,3-benzodioxoleHCID 74103—
반응물Methyl 2-cyano-3-ethoxy-2-propenoateHCID 101455—
반응물ButyllithiumHCID 178418339—
용매WaterHCID 962—
생성물(E)-2-cyano-3-(2,2-difluoro-1,3-benzodioxol-4-yl)-2-propenoic acid ethyl esterHCID 67735358—

반응 단계

53.3 g (337 mmol) of 2,2-difluoro-1,3-benzodioxole in 46 ml of toluene are metalated according to Example 2d), at from -15° to -10° C., with 137.8 g (409 mmol) of n-butyllithium solution (19.0% in toluene) in the presence of 39.3 g (339 mmol) of TMEDA. 69.1 g (409 mmol) of ethoxymethylenecyanoacetic acid methyl ester in 150 ml of toluene are metered in at from -15° to -10° C. over a period of 21/2 hours. The reaction mixture is added at +10° C. to 450 ml of water, the phases are separated and the organic phase is concentrated by evaporation in a vacuum rotary evaporator to yield the title compound.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US05420301
출처 데이터셋uspto-grants-1995_05
ORD IDord-61b678b9b6184ef6bc35ea82c07962dd
출처 메모uspto-grants-1995_05