反応 #40925

反応方程式

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

THF

→

title compound

3-{(1S,5R)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hex-3-yl}-1-propanol

溶媒

—

TEA

3-bromo-1-propanol

反応条件

後処理

1. 1
   温度the resulting mixture was heated
2. 2
   温度at reflux for 4 hours
3. 3
   workup.ADDITIONwas diluted with EtAcO (20 mL)
4. 4
   洗浄washed with water
5. 5
   乾燥dried over anhydrous Na2SO4
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他The crude product was purified by a silica SPE cartridge (10 g)
8. 8
   洗浄eluting with DCM/MeOH from 99/1 to 96/4

実験手順

To a solution of (1S,5R)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hexane (Prep4, 151 mg) in dry THF (3.3 mL), TEA (0.112 mL) and 3-bromo-1-propanol (0.073 mL) were added and the resulting mixture was heated at reflux for 4 hours. After cooling at room temperature it was diluted with EtAcO (20 mL), washed with water, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The crude product was purified by a silica SPE cartridge (10 g) eluting with DCM/MeOH from 99/1 to 96/4 to give the title compound as a colourless oil (143 mg).

出典