戻る
化工社化工社 化学情報印刷レポート · 研究参考用
HRID 256726作成日:2026年10月27日

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

https://huagongshe.com/reaction/256726

反応式

関与物質

役割名称HCID仕込み量
反応物Nitrosylsulfuric acidHCID 82157—
反応物4-Amino-3,5-dichlorobenzotrifluorideHCID 141094—
反応物4-Chloro-3-oxobutyryl chlorideHCID 3016262—
溶媒Acetic AcidHCID 176—
溶媒WaterHCID 962—
溶媒DichloromethaneHCID 6344—
生成物3-Chloropyruvaldehyde-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]hydrazoneHCID 131718235—

反応条件

温度0 °C

反応手順

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:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05258523
出典データセットuspto-grants-1993_11
ORD IDord-75618a1233cd4b9d896f8091605ff7dc
出典メモuspto-grants-1993_11