反应详情

To a stirred solution of 3-iodophenol (2.2 g, 10 mmol), N-(2-hydroxyethyl)morpholine (2 eq. 2.4 mL) and Ph3P (2 eq. 5.24 g) in THF (90 mL)at 0° C. was added dropwise a solution of diisopropylazodicarboxylate (2 eq. 3.96 g) in THF (20 mL). The resulting solution was stirred at room temperature overnight and was then quenched with NaHCO3. The product was extracted with EtOAc and the EtOAc layer was washed with NaCl (sat.), dried over sodium sulfate. The crude mixture was then purified on a silica gel column with 25% acetone in hexane to give 3-(2-morpholin-4-ylethyloxy)iodobenzene (2.8 g, 84% yield).

1. customwas then quenched with NaHCO3
2. extractionThe product was extracted with EtOAc
3. washthe EtOAc layer was washed with NaCl (sat.)
4. dry with materialdried over sodium sulfate
5. customThe crude mixture was then purified on a silica gel column with 25% acetone in hexane