반응 #4111

반응 방정식

9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-one

4-methylpiperidine

→

9-Methyl-6-(4-methyl-1-piperidinyl)-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine

용매

toluene

반응 조건

후처리

1. 1
   온도was heated under nitrogen until a solution
2. 2
   기타resulted
3. 3
   온도The mixture was heated
4. 4
   온도under reflux for three hours
5. 5
   여과filtered
6. 6
   기타the layers were separated
7. 7
   추출The aqueous phase was extracted with 250 ml of toluene
8. 8
   세척washed once with 2N sodium hydroxide solution, twice with water
9. 9
   건조dried over anhydrous sodium sulfate
10. 10
    여과filtered
11. 11
    농축concentrated in vacuo to 8.1 g (98%) of product
12. 12
    기타Recrystallization from ethyl acetate
13. 13
    기타provided the analytical sample, mp 194°-196° C.

실험 절차

A stirred mixture of 6.26 g (0.0250 mole) of 9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-one and 1000 ml of toluene was heated under nitrogen until a solution resulted. Then there was added 24.8 g (0.250 mole) of 4-methylpiperidine, followed by 14.2 g (0.075 mole) of titanium tetrachloride. The mixture was heated under reflux for three hours, cooled to room temperature and filtered. The filtrate was stirred with 500 ml of 2N sodium hydroxide solution for 15 minutes and the layers were separated. The aqueous phase was extracted with 250 ml of toluene. The toluene layers were combined, washed once with 2N sodium hydroxide solution, twice with water, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to 8.1 g (98%) of product. Recrystallization from ethyl acetate provided the analytical sample, mp 194°-196° C.

출처