反应详情

温度

60 °C

6-cyano-1H-benzopyrazole (14.3 g, 0.10 mol) was dissolved into 200 ml of 20% wt. sodium hydroxide, 3-chlorobromopropane (31.2 g, 0.20 mol) and tetrabutyl ammonium bromide (1.0 g) were added, and mixed for 5 min. The mixture was heated to 60° C., stirred to react for 2 hours. Then the reaction solution was cooled down to ambient temperature, 100 ml of dichloromethane was added for extraction and liquid separation. To the aqueous phase, 100 of dichloromethane was added for extraction. Organic phases were mixed, washed with 100 ml of saturated saline. Liquid was separated, and organic phase was evaporated to dryness to produce oily product. Oily products were separated and purified by chromatography with neutral Al2O3 to produce 13.9 g of 6-cyano-1-(3-chloropropyl)-1H-benzopyrazole, with a yield of 63.8%.

1. additionwere added
2. additionmixed for 5 min
3. customto react for 2 hours
4. temperatureThen the reaction solution was cooled down to ambient temperature
5. additionOrganic phases were mixed
6. washwashed with 100 ml of saturated saline
7. customLiquid was separated
8. customorganic phase was evaporated to dryness
9. customto produce oily product
10. customOily products were separated
11. custompurified by chromatography with neutral Al2O3