反应详情

Then, 9.1 g of N-(3-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)propyloxy)phthalimide was added to 150 ml of methanol, to which 1.9 g of hydrazine hydrate was added. The reaction mixture was stirred for 1 hour with heating under reflux, and returned to room temperature. To the reaction mixture was added 50 ml of water, from which the methanol was evaporated under reduced pressure. Further added were 15 ml of concentrated hydrochloric acid and 25 ml of water. The reaction mixture was stirred for 30 minutes with heating under reflux, returned to room temperature, and filtered. The crystals collected by filtration were added to 10% aqueous sodium hydrogencarbonate solution, and extracted with diethyl ether. The diethyl ether layer was washed with 10% aqueous sodium hydrogencarbonate solution and water. To this diethyl ether layer was added 3 ml of concentrated hydrochloric acid, and the mixture was concentrated and the dried, which afforded 6.8 g (yield, 92%) of O-(3-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)propyl)hydroxylamine hydrochloride, m.p., 171.8° C.

1. additionwas added
2. temperaturewith heating
3. temperatureunder reflux
4. customreturned to room temperature
5. customfrom which the methanol was evaporated under reduced pressure
6. additionFurther added
7. stirringThe reaction mixture was stirred for 30 minutes
8. temperaturewith heating
9. temperatureunder reflux
10. customreturned to room temperature
11. filtrationfiltered
12. filtrationThe crystals collected by filtration
13. additionwere added to 10% aqueous sodium hydrogencarbonate solution
14. extractionextracted with diethyl ether
15. washThe diethyl ether layer was washed with 10% aqueous sodium hydrogencarbonate solution and water
16. additionTo this diethyl ether layer was added 3 ml of concentrated hydrochloric acid
17. concentrationthe mixture was concentrated