反应详情

According to Scheme 3, step 3: A mixture of 4,6-Difluoro-2-methyl-indan-1-ol (8a) (0.65 g, 3.53 mmol) and para-toluene sulfonic acid monohydrate (30 mg, 0.18 mmol) in toluene was heated at reflux for 1 h. The solution was washed with aqueous saturated NaHCO3 and brine, dried over MgSO4 and solvents evaporated. The crude product was purified by silica gel chromatography (eluting with 0% to 100% ethyl acetate in heptane to give 0.50 g of 5,7-Difluoro-2-methyl-1H-indene (9a) which was used immediately in the next step.

1. temperaturewas heated
2. temperatureat reflux for 1 h
3. washThe solution was washed with aqueous saturated NaHCO3 and brine
4. dry with materialdried over MgSO4 and solvents
5. customevaporated
6. customThe crude product was purified by silica gel chromatography (
7. washeluting with 0% to 100% ethyl acetate in heptane