Reacción #3689

Ecuación de reacción

ethyl acetate hexane

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

dimethylamine

1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone

→

beige solid

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

Disolventes

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe methanol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   LavadoThe resulting solid is washed with water
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   Lavadothe organic layer washed with saturated NaHCO3, brine
6. 6
   Secadodried with Na2SO4
7. 7
   FiltraciónThe mixture is filtered
8. 8
   Otrothe filtrate evaporated in vacuo
9. 9
   Otroto give a residue which

Procedimiento

A partial solution of ?? g of α-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide in 1 ml of methanol is treated with 0.5 ml of dimethylamine and 1 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and stirring continued for 20 hours. The methanol is evaporated and the residue diluted with water. The resulting solid is washed with water, dissolved in ethyl acetate and the organic layer washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to give a residue which is stirred with ethyl acetate-hexane to give 0.15 g of a beige solid. MS(CI): 465 (M+H).

Fuente