反应详情

A solution of compound 208A (62 mg, 0.32 mmol) in 1 mL EtOH containing 0.1 mL 12 N HCl was heated to reflux. Iron powder (62 mg, 1.11 mmol) was added in small portions and heating was continued for 2 h. The mixture was cooled, neutralized with 1 N NaOH solution and the aqueous layer was extracted with CH2Cl2. The combined organic phases were dried over MgSO4 and concentrated in vaccuo to leave a residue which was purified by flash chromatography on silica gel eluting with 40 to 80% EtOAc in hexanes to give 42 mg (0.26 mmol, 80%) of compound 208B as a yellow solid.

1. temperatureheating
2. temperatureThe mixture was cooled
3. extractionthe aqueous layer was extracted with CH2Cl2
4. dry with materialThe combined organic phases were dried over MgSO4
5. concentrationconcentrated in vaccuo
6. customto leave a residue which
7. customwas purified by flash chromatography on silica gel eluting with 40 to 80% EtOAc in hexanes