反应详情

To a solution of 267 (35 mg, 0.13 mmol) in AcOH (1 mL) at 90° C., was added iron powder (36 mg, 0.65 mmol). The reaction mixture was stirred vigorously for 10 min, cooled, filtered through a Celite pad and concentrated. The residue was partitioned between DCM and NaHCO3 saturated solution. Phases were separated; the aqueous phase was neutralized with AcOH and extracted with DCM. Primary organic phase and the extract were combined and concentrated to give the title compound 268 (31 mg, 99%) as an off-white solid. MS (m/z): 244.1(M+H) (found).

1. temperaturecooled
2. filtrationfiltered through a Celite pad
3. concentrationconcentrated
4. customThe residue was partitioned between DCM and NaHCO3 saturated solution
5. customPhases were separated
6. extractionextracted with DCM
7. concentrationconcentrated