反应详情

温度

0 °C

To 5.7 g (0.023 mol) of Boc-PheOH dissolved in THF (30 mL) at −10° C. under N2 are added NMM (2.5 mL, 0.023 mol) and IBCF (3 mL, 0.023 mol). The reaction mixture is stirred for 15 minutes and filtered. The filtrate is slowly added to an ice-cold solution of NaBH4 (2.3 g, 0.061 mol) in H2O (10 mL) and then stirred for 1 hour at ice-bath temperature followed by stirring for 1 hour at room temperature. The reaction is cooled to 0° C., treated with saturated NaHCO3 solution, extracted with EtOAc, washed with 1M HCl, washed with water, dried over anhydrous MgSO4, and evaporated to dryness. The crude product is purified over a silica gel column eluted with 95:5 EtOAc/MeOH.

1. filtrationfiltered
2. stirringstirred for 1 hour at ice-bath temperature
3. stirringby stirring for 1 hour at room temperature
4. extractionextracted with EtOAc
5. washwashed with 1M HCl
6. washwashed with water
7. dry with materialdried over anhydrous MgSO4
8. customevaporated to dryness
9. customThe crude product is purified over a silica gel column
10. washeluted with 95:5 EtOAc/MeOH