反应详情

Dissolved 4-(5-nitro-2-pentafluoroethyl-phenoxymethyl)-piperidine (646 mg) in 1,2-dichloroethane (6.4 ml), then added acetone (136 ul), NaBH(OAc)3 (541 mg) and finally acetic acid (105 ul). Stirred the cloudy yellow solution under N2 at RT overnight. Added another 130 uL acetone and stirred at RT over weekend. Quenched the reaction with 30 mL N NaOH/H2O and stirred 10 min. Extracted with Et2O and the organic layer was brine-washed, dried over Na2SO4, filtered and concentrated in vacuo. Dried under high vacuum for several h to obtain 1-isopropyl-4-(5-nitro-2-pentafluoroethyl-phenoxymethyl)-piperidine as a yellow orange solid.

1. stirringstirred at RT over weekend
2. customQuenched
3. customthe reaction with 30 mL N NaOH/H2O
4. stirringstirred 10 min
5. extractionExtracted with Et2O
6. washwashed
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customDried under high vacuum for several h