反应详情

The product of Example 12 (627 mg, 1.46 mmol) was added to a freshly prepared solution of sodium methoxide in methanol (1.5 equivalents sodium in 5 mL methanol) in dry dimethylformamide (3-5 mL) and the mixture was stirred at room temperature for 15-30 minutes. The reaction mixture was diluted with water and extracted with ethyl acetate (3x). The combined organic extracts were washed with water, brine, dried (MgSO4) and concentrated in vacuo. The crude residue (0.64 g) was purified by chromatography (Silica Gel 60, first with 2% methanol in methylene chloride followed by 5% ethyl acetate in methylene chloride) to give pure title compound (308 rag) as a colorless oil which crystallized from methanol, mp 64.5°-65.5° C. (white solid).

1. extractionextracted with ethyl acetate (3x)
2. washThe combined organic extracts were washed with water, brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe crude residue (0.64 g) was purified by chromatography (Silica Gel 60