تفاعل #4128

معادلة التفاعل

N-bromosuccinimide

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

dichloromethane

→

product

المردود 11.6%

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

المردود 11.6%

المذيبات

dimethylformamide

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   غسيلwas washed with brine (4 times, 150 ml)
2. 2
   تجفيفdried over anhydrous magnesium sulfate
3. 3
   أخرىThe solvent was removed at reduced pressure
4. 4
   أخرىthe residue was dried
5. 5
   أخرىPurification
6. 6
   غسيلeluted with dichloromethane (500 ml) and 2% methanol in dichloromethane (250 ml)
7. 7
   workup.ADDITIONThe fractions containing the product
8. 8
   تركيزconcentrated
9. 9
   أخرىRecrystallization from 2-propanol:water (1:1, 20 ml)

الإجراء التجريبي

A solution of N-bromosuccinimide (0.91 g, 5.1 mmoles) in dimethylformamide (3 ml) was added dropwise to a solution of 6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (1.6 g, 4.8 mmoles) in dimethylformamide (30 ml) at 0°-3° C. The reaction mixture was stirred for 30 minutes. The solution was poured into dichloromethane (250 ml), and was washed with brine (4 times, 150 ml), and dried over anhydrous magnesium sulfate. The solvent was removed at reduced pressure and the residue was dried. Purification was accomplished by flash chromatography on an aluminium oxide column (grade III, 60 g), eluted with dichloromethane (500 ml) and 2% methanol in dichloromethane (250 ml). The fractions containing the product were pooled and concentrated. Recrystallization from 2-propanol:water (1:1, 20 ml) yielded 230 mg (11.6%) of product, mp 177°-177° C.

المصدر