反应 #41051

反应方程式

dioxane

1-(3-chloro-propyl)-5-pyridin-3-yl-1H-pyrimidine-2,4-dione

(1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane

DIPEA

→

HCl

title compound

5-(3-pyridinyl)-1-(3-{(1S,5R)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hex-3-yl}propyl)-2,4(1H,3H)-pyrimidinedione dihydrochloride

溶剂

EtOH

反应条件

后处理

1. 1
   其他irradiated at 130° C. for 3 hours
2. 2
   其他The solvent was removed under vacuum
3. 3
   其他the residue was partitioned between water and ethyl acetate
4. 4
   干燥The organic phase was dried (Na2SO4)
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他The residue was purified by preparative LC-MS

实验过程

A solution of 1-(3-chloro-propyl)-5-pyridin-3-yl-1H-pyrimidine-2,4-dione (Prep43, 92 mg, 0.34 mmol), (1S,5R)-1-(4-trifluoromethyl-phenyl)-3-aza-bicyclo[3.1.0]hexane (Prep4, 68 mg, 0.34 mmol), and DIPEA (134 μl, 1 mmol) in absolute EtOH (3 mL) was placed in a microwave oven and irradiated at 130° C. for 3 hours. The solvent was removed under vacuum and the residue was partitioned between water and ethyl acetate. The organic phase was dried (Na2SO4), filtered and evaporated. The residue was purified by preparative LC-MS. After treatment with 4N HCl in dioxane (2 eq), the title compound was obtained (5 mg, 4% yield)

来源