تفاعل #3686

معادلة التفاعل

4-[(2-methylbenzoyl)amino]-3-chlorobenzoyl chloride

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

N,N-diisopropylethylamine

→

product

المردود 106.0%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)-2-chlorophenyl]-2-methylbenzamide

المردود 106.0%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with H2O and saturated NaHCO3
2. 2
   تجفيفThe organic layer is dried (Na2SO4)
3. 3
   تركيزThe filtrate is concentrated
4. 4
   workup.DISSOLUTIONthe residue (4.0 g) dissolved in dichloromethane
5. 5
   ترشيحagain filtered through a pad of hydrous magnesium silicate
6. 6
   أخرىThe filtrate is evaporated

الإجراء التجريبي

To a mixture of 1.38 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 1.11 g of N,N-diisopropylethylamine in 50 ml of dichloromethane is added 2.61 g of 4-[(2-methylbenzoyl)amino]-3-chlorobenzoyl chloride in 25 ml of dichloromethane. The mixture is stirred at room temperature overnight and then washed with H2O and saturated NaHCO3. The organic layer is dried (Na2SO4) and passed through a pad of hydrous magnesium silicate. The filtrate is concentrated, the residue (4.0 g) dissolved in dichloromethane and again filtered through a pad of hydrous magnesium silicate. The filtrate is evaporated to give the product as a glass (3.62 g). A 1.8 g sample of the glass is crystallized from ethyl acetate to give 1.4 g of crystals, m.p. 176°-178° C.

المصدر