反应详情

温度

0 °C

A mechanically stirred solution of potassium tert-butoxide in tert-butanol (1 M, 203 mL) under a nitrogen atmosphere was treated with anhydrous ether (125 mL), cooled to 0° C., treated with the product from Example 84B (15.5 g, 97 mmol) in ether (55 mL) over 2 minutes, stirred for 10 minutes and then treated with 2M HCl (240 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate (2×, 200 mL). The combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated. The residue was purified on silica gel eluting with ethyl acetate:formic acid:water:hexane (200:1:1:200) to provide the title compound.

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with ethyl acetate (2×, 200 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified on silica gel eluting with ethyl acetate:formic acid:water:hexane (200:1:1:200)