Reaktion #3689

Reaktionsgleichung

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

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe methanol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   WaschenThe resulting solid is washed with water
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   Waschenthe organic layer washed with saturated NaHCO3, brine
6. 6
   Trocknendried with Na2SO4
7. 7
   FiltrationThe mixture is filtered
8. 8
   Sonstigethe filtrate evaporated in vacuo
9. 9
   Sonstigeto give a residue which

Vorschrift

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).

Quelle