反应详情

Into a 100-mL round-bottom flask, was placed a solution of tert-butyl 2-(5-(methoxycarbonyl)-2,4-dimethylphenyl)-4,5,7,8-tetrahydroimidazo[4,5-d]azepine-6(1H)-carboxylate (compound 83.3, 800 mg, 2.00 mmol) in dichloromethane (16 mL). Trifluoroacetic acid (4 mL) was added drop-wise and the resulting solution was stirred for 5 h at room temperature. The pH of the solution was carefully adjusted to 8-9 with NaHCO3 (sat.) and the aqueous phase was extracted with DCM (3×30 mL), and the combined organics were dried (Na2SO4), filtered, and concentrated under reduced pressure to yield 0.60 mg (crude) of the title compound as brown oil.

1. customInto a 100-mL round-bottom flask, was placed
2. extractionthe aqueous phase was extracted with DCM (3×30 mL)
3. dry with materialthe combined organics were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure