反应详情

The solution of 12-2 (0.3 g, 0.92 mmol) in 25 mL of acetic acid was heated to 80° C. for 8 h. The volatile was removed in vacuo and the residue was neutralized with Na2CO3 solution to pH:7. The mixture was extracted with ethyl acetate (100 mL) and washed with brine. The organic layer was dried over anhydrous Na2SO4. After filtration and concentration, a residue was obtained, which was purified by preparative TLC to give 12-3 (68 mg, 23.9%)

1. customThe volatile was removed in vacuo
2. extractionThe mixture was extracted with ethyl acetate (100 mL)
3. washwashed with brine
4. dry with materialThe organic layer was dried over anhydrous Na2SO4
5. filtrationAfter filtration and concentration
6. customa residue was obtained
7. customwhich was purified by preparative TLC