反应详情

A solution of 32 (1.5 g, 3.96 mmol) in anhydrous tetrahydrofuran (16 mL) was stirred under nitrogen at room temperature and 1M ortho-methoxyphenyl magnesium bromide in tetrahydrofuran (6 mL, 1.5 equiv.) was slowly added. Stirring was continued at room temperature for 30 min and at 60° C. for 3 hr. After cooling, the reaction mixture was poured on saturated ammonium chloride (100 mL) and extracted with ethyl acetate (150 mL). The organic extract was washed with water (2×100 mL), dried over sodium sulfate and filtered. The solvent was removed in a rotary evaporator and the crude 33 thus obtained was used in the next step without further purification.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate (150 mL)
3. extractionThe organic extract
4. washwas washed with water (2×100 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customThe solvent was removed in a rotary evaporator
8. customthe crude 33 thus obtained
9. customwas used in the next step without further purification