반응 #4107

반응 방정식

N-propylpiperazine

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

sodium hydroxide

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product

수율 30.1%

9-Bromo-6-(4-n-propyl-1-piperazinyl)-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine

수율 30.1%

용매

toluene

반응 조건

후처리

1. 1
   온도was heated until a solution
2. 2
   기타resulted
3. 3
   온도The mixture was refluxed for 3 hours
4. 4
   기타the layers were separated
5. 5
   추출The aqueous phase was extracted with 300 ml of toluene
6. 6
   여과filtered
7. 7
   세척washed once with 2N sodium hydroxide solution, twice with water
8. 8
   건조dried over anhydrous sodium sulfate
9. 9
   농축concentrated to an oily solid
10. 10
    workup.DISSOLUTIONThe oily solid was dissolved in 25 ml of hot ethyl acetate
11. 11
    여과filtered
12. 12
    기타to crystallize first at room temperature

실험 절차

A stirred mixture of 7.88 g (0.0250 mole) of 9-bromo-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-one and 1200 ml of toluene was heated until a solution resulted. Then there was added 32.1 g (0.25 mole) of N-propylpiperazine, followed by 14.2 g (0.075 mole) of titanium tetrachloride. The mixture was refluxed for 3 hours, and then cooled to room temperature. The mixture was stirred with 500 ml of 2N sodium hydroxide solution for 15 minutes and the layers were separated. The aqueous phase was extracted with 300 ml of toluene. The toluene layers were combined, filtered, washed once with 2N sodium hydroxide solution, twice with water, dried over anhydrous sodium sulfate, and concentrated to an oily solid. The oily solid was dissolved in 25 ml of hot ethyl acetate, filtered, and allowed to crystallize first at room temperature, then at 0° C. to yield 3.20 g (30%) of product, mp 134°-136° C.

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