反应详情

A solution of 17-1 (9 g, 28 mmol), potassium hydroxide (2.36 g, 42 mmol) and methyl iodide (6 g, 42 mmol) in DMF (30 mL) was stirred at room temperature for 2 h. The mixture was poured into water (50 mL), extracted with ethyl acetate (3×50 mL). The extracts were washed with water (3×50 mL) and brine (2×50 mL), dried over MgSO4, filtered, and evaporated to afford 33-3 (8 g, 90%) which was used directly in next step. LRMS: calc 333.0 and found: 334.0 [M+1].

1. extractionextracted with ethyl acetate (3×50 mL)
2. washThe extracts were washed with water (3×50 mL) and brine (2×50 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated