반응 #3689

반응 방정식

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

용매

methanol

반응 조건

후처리

1. 1
   기타The methanol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   세척The resulting solid is washed with water
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   세척the organic layer washed with saturated NaHCO3, brine
6. 6
   건조dried with Na2SO4
7. 7
   여과The mixture is filtered
8. 8
   기타the filtrate evaporated in vacuo
9. 9
   기타to give a residue which

실험 절차

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).

출처