تفاعل #3687

معادلة التفاعل

(±)-2-chloro-2-phenylacetyl chloride

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

triethylamine

→

pink solid

المردود 106.9%

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

المردود 106.9%

المذيبات

NaHCO3

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىThe methylene chloride is evaporated
2. 2
   استخلاصthe residue is extracted with ethyl acetate
3. 3
   غسيلThe separated organic layer is washed with saturated NaHCO3 and brine
4. 4
   تجفيفdried with Na2SO4
5. 5
   ترشيحby filtering through a pad of hydrous magnesium silicate
6. 6
   أخرىThe filtrate is evaporated to a residue which
7. 7
   workup.STIRRINGis stirred with ether-hexane

الإجراء التجريبي

To a solution of 0.61 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 8 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.47 g of (±)-2-chloro-2-phenylacetyl chloride in 2 ml of methylene chloride. The mixture is stirred at room temperature for 1 hour and then diluted with 10 ml of 50% NaHCO3. The methylene chloride is evaporated and the residue is extracted with ethyl acetate. The separated organic layer is washed with saturated NaHCO3 and brine and then dried with Na2SO4 followed by filtering through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is stirred with ether-hexane to give 0.98 g of pink solid. MS(CI): 456(M+H).

المصدر