반응 #55367

반응 방정식

HCl

1-methyl-4-(3-bromo-5-hydroxy-5H-dibenzo[a,d]cyclohepten-5-yl)piperidine

trifluoroacetic acid

(±)-1-methyl-4-(3-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine hydrochloride

trifluoroacetic anhydride

→

(±)-1-methyl-4-(3-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine

용매

ethanol

반응 조건

후처리

1. 1
   온도refluxed for 16 hours
2. 2
   기타The solvents are removed by evaporation on a rotary evaporator
3. 3
   workup.DISSOLUTIONThe residue is dissolved in chloroform
4. 4
   세척this chloroform solution is washed with sodium hydroxide solution, water
5. 5
   건조dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   기타Evaporation of the chloroform from the filtrate
8. 8
   기타gives 0.88 g
9. 9
   온도is cooled
10. 10
    기타The white crystalline material that precipitates
11. 11
    여과is collected by filtration
12. 12
    기타is recrystallized from acetonitrile
13. 13
    기타to give 0.67 g

실험 절차

A solution of 0.86 g. (0.003 mol) of 1-methyl-4-(3-bromo-5-hydroxy-5H-dibenzo[a,d]cyclohepten-5-yl)piperidine in 30 ml. of trifluoroacetic acid and 15 ml. of trifluoroacetic anhydride is stirred and refluxed for 16 hours. The solvents are removed by evaporation on a rotary evaporator. The residue is dissolved in chloroform, and this chloroform solution is washed with sodium hydroxide solution, water, dried over magnesium sulfate, and filtered. Evaporation of the chloroform from the filtrate gives 0.88 g. of a yellow oil. This oil is dissolved in a minimum amount of absolute ethanol, treated with ethanolic HCl, and is cooled. The white crystalline material that precipitates is collected by filtration and is recrystallized from acetonitrile to give 0.67 g. of (±)-1-methyl-4-(3-bromo-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine hydrochloride.

출처