反应详情

43.5 gm (0.144 mol) of 1-benzyl-4-chloro-2,3,6,7-tetrahydro-5-oximinomethylene-1H-azepine hydrochloride were added to 450 ml of phosphorus oxychloride while stirring at ambient temperature. The mixture was then stirred for 3 hours more, and the reaction mixture was then allowed to stand overnight. Then, the excess phosphorus oxychloride was distilled off in a rotary evaporator, and the residue was carefully mixed with water while cooling with ice. While cooling was continued, the mixture was made slightly alkaline by the addition of concentrated ammonia, and an oil separated out which crystallized when scratched. The crystal slurry thus obtained was suction-filtered, washed with water, dried and recrystallized from isopropyl alcohol.

1. stirringThe mixture was then stirred for 3 hours more
2. distillationThen, the excess phosphorus oxychloride was distilled off in a rotary evaporator
3. additionthe residue was carefully mixed with water
4. temperaturewhile cooling with ice
5. temperatureWhile cooling
6. additionthe mixture was made slightly alkaline by the addition of concentrated ammonia
7. customan oil separated out which
8. customcrystallized when
9. customThe crystal slurry thus obtained
10. filtrationwas suction-filtered
11. washwashed with water
12. customdried
13. customrecrystallized from isopropyl alcohol