反应 #4111

反应方程式

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

溶剂

toluene

反应条件

后处理

1. 1
   温度was heated under nitrogen until a solution
2. 2
   其他resulted
3. 3
   温度The mixture was heated
4. 4
   温度under reflux for three hours
5. 5
   过滤filtered
6. 6
   其他the layers were separated
7. 7
   萃取The aqueous phase was extracted with 250 ml of toluene
8. 8
   洗涤washed once with 2N sodium hydroxide solution, twice with water
9. 9
   干燥dried over anhydrous sodium sulfate
10. 10
    过滤filtered
11. 11
    浓缩concentrated in vacuo to 8.1 g (98%) of product
12. 12
    其他Recrystallization from ethyl acetate
13. 13
    其他provided the analytical sample, mp 194°-196° C.

实验过程

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.

来源