反应详情

To a stirred solution of o-methylcinnamic acid (Intermediate-1) (30 g, 185 mmol) in dry THF (100 mL) was added TEA (51.5 mL, 37 mmol) and diphenylphosphoryl azide (DPPA) (56 g, 204 mmol) slowly under N2 atmosphere and the mixture was stirred at room temperature for 2-3 h. It was quenched with cold water, extracted with EtOAc (3×200 mL), washed with water (2×200 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to give the crude product. It was recrystallized from MeOH to obtain the desired compound (23 g, 66%).

1. customIt was quenched with cold water
2. extractionextracted with EtOAc (3×200 mL)
3. washwashed with water (2×200 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customto give the crude product
8. customIt was recrystallized from MeOH