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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 256726생성일: 2026년 10월 26일

Nitrosylsulfuric acid → 3-Chloropyruvaldehyde-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]hydrazone

https://huagongshe.com/reaction/256726

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참여 물질

역할이름HCID투입량
반응물Nitrosylsulfuric acidHCID 82157—
반응물4-Amino-3,5-dichlorobenzotrifluorideHCID 141094—
반응물4-Chloro-3-oxobutyryl chlorideHCID 3016262—
용매Acetic AcidHCID 176—
용매WaterHCID 962—
용매DichloromethaneHCID 6344—
생성물3-Chloropyruvaldehyde-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]hydrazoneHCID 131718235—

반응 조건

온도0 °C

반응 단계

144.3 g of 4-(trifluoromethyl)-2,6-dichloroaniline (96 percent) was dissolved in 120 ml of acetic acid and mixed within one hour at 20° C. with 209.7 g of nitrosylsulfuric acid (40 percent in sulfuric acid monohydrate). Then the reaction mixture was cooled to 0° C. and diluted with 480 ml of water. This solution was instilled in a solution of 111.6 g of γ-chloroacetoacetyl chloride in 400 ml of dichloromethane (produced according to Swiss Patent No. 642,611) at -5° to 0° C. within one hour. The mixture was stirred for one more hour at 10° C., and then the phases were separated. The aqueous phase was extracted with 100 ml of dichloromethane, the combined organic phase concentrated by evaporation and the residue suspended with 300 ml of cyclohexane. The undissolved solid was filtered off, washed two times each with 100 ml of cyclohexane and dried at 40 torr. The yield of the product was 183.6 g of ochre crystals. Data concerning the product was:

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US05258523
출처 데이터셋uspto-grants-1993_11
ORD IDord-75618a1233cd4b9d896f8091605ff7dc
출처 메모uspto-grants-1993_11