反应详情

温度

120 °C

In a 0.5/2 mL sealed MW vial (1S,5R)-3-(3-chloropropyl)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hexane (Prep5, 62.6 mg, 0.206 mmol) was dissolved in Dimethyl Sulfoxide (DMSO) (0.8 ml), and, 6-hydroxy-5-(3-methyl-1,2,4-oxadiazol-5-yl)-2(1H)-pyrimidinone (Prep33, 40 mg, 0.206 mmol), Sodium iodide (46.3 mg, 0.309 mmol) and Dipea (0.126 mL, 0.721 mmol) were then added. The red mixture so obtained was heated at 120° C. for 4 h, then left at 80° C. overnight. The day after DIPEA (0.054 mL, 0.310 mmol) was added and the mixture and the heated at 120° C. for further 4 h. The mixture was treated with EtOAc and washed with NH4Cl sat. sol. The organic phase was dried over Na2SO4 anhydrous, filtered and evaporated under reduced pressure providing a brown residue. The crude was purified first by SCX cartridge and then by Biotage Si 12+M cartridge with a gradient of DCM/DCM/MeOH (9:1). 19 mg of the title compound were obtained as a yellow oil.

1. customThe red mixture so obtained
2. temperaturethe mixture and the heated at 120° C. for further 4 h
3. washwashed with NH4Cl sat. sol. The organic phase
4. dry with materialwas dried over Na2SO4 anhydrous
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customproviding a brown residue
8. customThe crude was purified first by SCX cartridge