Methyl iodide → HCID 67246011, compound

Participants

Reaction Steps

To a vigorously stirred solution of the compound of example 41e (4.5 g; 12.7 mmol) in dry DMF (20 ml) was added sequentially fused K2CO3 (3.5 g; 25.5 mmol), methyl iodide (0.96 ml; 15.3 mmol) and KF (0.45 g). The reaction mixture was stirred for 3 h, diluted with water (200 ml) and the oily residue was extracted with chloroform (3×30 ml). The organic layer was washed with brine, dried (Na2SO4), concentrated and purified using flash chromatography (silica gel, 3% CH3CN in chloroform). Yield, 3.25 g (69.5%); mp, 75° C.; MS (ESI+): 390 (M++Na), 368 (M++1); analysis: C18H25NO7 requires C, 58.85; H, 6.85; N, 3.81. found: C, 58.79; H, 7.26; N, 3.81%.

Provenance & Evidence