反应 #3689

反应方程式

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

溶剂

methanol

反应条件

后处理

1. 1
   其他The methanol is evaporated
2. 2
   workup.ADDITIONthe residue diluted with water
3. 3
   洗涤The resulting solid is washed with water
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   洗涤the organic layer washed with saturated NaHCO3, brine
6. 6
   干燥dried with Na2SO4
7. 7
   过滤The mixture is filtered
8. 8
   其他the filtrate evaporated in vacuo
9. 9
   其他to give a residue which

实验过程

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).

来源