Реакция #3689

Уравнение реакции

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

Растворители

methanol

Условия реакции

Обработка

1. 1
   ДругоеThe methanol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   ПромывкаThe resulting solid is washed with water
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   Промывкаthe organic layer washed with saturated NaHCO3, brine
6. 6
   Сушкаdried with Na2SO4
7. 7
   ФильтрацияThe mixture is filtered
8. 8
   Другоеthe filtrate evaporated in vacuo
9. 9
   Другоеto give a residue which

Методика

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).

Источник