反应详情

To a solution of 2-iodo-3-(methyloxy)phenol (Intermediate 47, 10.3 g) in DMF (100 ml, SCRC) was added NaH (60%, wt., 1.977 g, 49.4 mmol) portionwise. The reaction mixture was stirred at room temperature for 1 hour and 3-chloro-2-methyl-1-propene (3.73 g, 41.2 mmol, Aldrich) was added. The resulting mixture was stirred at room temperature for 2 hours and water (50 ml) was added. The reaction mixture was extracted with ethyl acetate (3 times 200 ml, SCRC) and the combined organic layer were dried, evaporated and purified by silica gel chromatography with as eluents EtOAc/PE (1/30) to afford the title compound as a yellow liquid (11.6 g)

1. stirringThe resulting mixture was stirred at room temperature for 2 hours
2. extractionThe reaction mixture was extracted with ethyl acetate (3 times 200 ml, SCRC)
3. customthe combined organic layer were dried
4. customevaporated
5. custompurified by silica gel chromatography with as eluents EtOAc/PE (1/30)