Method for synthesizing prochloraz intermediate
A synthesis method and intermediate technology, applied in the field of prochloraz intermediate N-[2-ethyl]-N-n-propylamine, can solve the problems of shortened reaction time, low yield, long amination reaction cycle, etc. , achieve the effects of shortening the reaction time, saving costs, and eliminating vacuum distillation operations
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Embodiment 1
[0032] Take 26g of 2-(2,4,6-trichlorophenoxy)chloroethane in a 250mL three-necked flask, add 25mL of n-propylamine and 50mL of freshly prepared ionic liquid, reflux at 80°C, track and detect with TLC, and react for 2h completely, cooled to room temperature, washed 3 times with 300mL water, filtered to obtain filter cake and filtrate, and dried the filter cake to obtain the product N-[2-(2,4,6-trichlorophenoxy)ethyl]- N-n-propylamine 27.8g, yield 98%, purity 99.2% (detected by liquid chromatography).
Embodiment 2
[0034] Take 26g of 2-(2,4,6-trichlorophenoxy)chloroethane into a 250mL three-necked flask, add 15mL of n-propylamine and 26mL of freshly prepared ionic liquid, reflux at 80°C, track and detect with TLC, and react for 3h completely, cooled to room temperature, washed 3 times with 300mL water, filtered to obtain filter cake and filtrate, and dried the filter cake to obtain the product N-[2-(2,4,6-trichlorophenoxy)ethyl]- N-n-propylamine 26.2g, yield 93%, purity 99.0% (detected by liquid chromatography).
Embodiment 3
[0036] Take 26g of 2-(2,4,6-trichlorophenoxy)chloroethane in a 250mL three-necked flask, add 50mL of n-propylamine and 78mL of newly prepared ionic liquid, reflux at 80°C, track and detect with TLC, and react for 2h completely, cooled to room temperature, washed 3 times with 300mL water, filtered to obtain filter cake and filtrate, and dried the filter cake to obtain the product N-[2-(2,4,6-trichlorophenoxy)ethyl]- N-n-propylamine 27.5g, yield 97%, purity 99.5% (detected by liquid chromatography).
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