Methyl iodide → HCID 44553220, compound

Participants

Reaction Steps

To the product of Step 4 (0.38 g, 0.96 mmol) and iodomethane (1.0 mL, 1M solution in THF, 1.0 mmol) in THF (5 mL) at 5° C. under argon was added NaH (60% in mineral oil, 0.040 g, 1.0 mmol). After stirring at RT for 16 h, the reaction was partitioned between CH2Cl2 (10 mL) and H2O (20 mL). The organic layer was separated, washed with H2O, brine, dried with anhydrous Na2SO4 and concentrated. The residue was purified by crystallization from EtOAc/hexane to give the title compound. 1H NMR (400 MHz, CDCl3): 2.52 (3H, s), 3.03 (3H, s), 3.51 (3H, s), 6.91-6.99 (2H, m), 7.21-7.29 (2H, m), 7.88-7.94 (2H, m), 8.21-8.27 (2H, m). LC-MS: m/z 393.0 [M+H]+

Provenance & Evidence