反应详情

Ethyl 2-chlorobenzimidate (2.80 g) and triethylamine (1.70 g) are dissolved in toluene (50 ml), to which is added dropwise (E)-3-chloro-2-methyl-2-butenoyl chloride at 5° C.-10° C. with stirring, and the stirring is continued at room temperature for 4 hours after the completion of the addition. After the completion of the reaction, the reaction mixture is added with toluene (150 ml), washed with a saline solution, dried on anhydrous magnesium sulfate and concentrated under a reduced pressure. The concentrate is purified through a silica gel column chromatography (Wakogel C-200: made by Wako Junyaku Kabushiki Kaisha) using a mixed solution of hexane-ethyl acetate (10:1) as a developing medium to obtain an oily ethyl (E)-N-(3-chloro-1-methyl-2-butenoyl)-2-chlorobenzimidate (2.37 g).

1. additionafter the completion of the addition
2. customAfter the completion of the reaction
3. washwashed with a saline solution
4. dry with materialdried on anhydrous magnesium sulfate
5. concentrationconcentrated under a reduced pressure
6. customThe concentrate is purified through a silica gel column chromatography (Wakogel C-200: made by Wako Junyaku Kabushiki Kaisha)