反应 #3588

反应方程式

2-chlorobenzoyl chloride

10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

→

desired product

收率 72.1%

N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2-chlorobenzamide

收率 72.1%

溶剂

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   其他The bath is removed
2. 2
   workup.STIRRINGthe reaction mixture stirred at room temperature for 18 hours
3. 3
   浓缩The volatiles are concentrated in vacuo
4. 4
   其他to give a residue which
5. 5
   洗涤washed with water, 2N citric acid, 1M NaHCO3 and brine
6. 6
   干燥The organic layer is dried with Na2SO4
7. 7
   过滤filtered
8. 8
   浓缩concentrated in vacuo
9. 9
   其他to give a residue which
10. 10
    其他is crystallized from methylene chloride

实验过程

To a solution of 347 mg of 2-chlorobenzoyl chloride in 5 ml of methylene chloride at 0° C. is added 346 μl of triethylamineo After stirring for 3 minutes, 500 mg of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added. The bath is removed and the reaction mixture stirred at room temperature for 18 hours. The volatiles are concentrated in vacuo to give a residue which is dissolved in methylene chloride, washed with water, 2N citric acid, 1M NaHCO3 and brine. The organic layer is dried with Na2SO4, filtered and concentrated in vacuo to give a residue which is crystallized from methylene chloride to give 525 mg of the desired product as a white crystalline solid, m.p. 228°-230° C.

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