Methyl iodide → HCID 13911212, compound

Participants

Reaction Steps

A solution containing compound 1 (15.0 g, 55.4 mmol), K2CO3 (20.0 g, 0.145 mol) and CH3I (30 mL, 0.48 mol) in 250 mL acetone was refluxed for 6 hours. The solvent was evaporated and the residue partitioned between CH2Cl2 and H2O. The organic layer was dried over Na2SO4, filtered and evaporated to leave a yellow-white powder. Recrystallization from CH3OH/pet ether at -20° C. gave 14.9 g of white crystals (94%) Tee material was characterized by NMR, TLC, mass spectroscopy, IR and elemental analysis, m.p. 131°-132.5° C. Anal. Calcd. for C16H15NO4 : C, 67.35; H, 5.31; N, 4.91. Found: C, 67.54; H, 5.38; N, 4.87.

Provenance & Evidence