反应详情

温度

0 °C

The title compound of Example 26 (1.0 g., 3.2 mmol.) was dissolved at 0° C. under argon in 2.5 mL of a 1:1 concentrated NH4OH:H2O solution. The reaction mixture was stirred at 0° C. for minutes and then acidified with 5N HCl to pH 6 at 0° C. The product was extracted with ethyl acetate containing 5 percent methanol (3×) (200 mL portions). The organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was chromatographed through 50 g of Merck silica gel using a (3:3:94) methanol:acetic acid:methylene chloride solvent system. The appropriate fractions were combined and concentrated to yield 0.56 g of the title product, m.p. 182°-184° C.

1. extractionThe product was extracted with ethyl acetate containing 5 percent methanol (3×) (200 mL portions)
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was chromatographed through 50 g of Merck silica gel using a (3:3:94) methanol
6. concentrationconcentrated