Methyl iodide → HCID 52933898, compound

Participants

Reaction Steps

To a solution of example 1 (48 mg. 0.13 mmol) in DMF (6 mL), 55-65% NaH dispersion in mineral oil (7.3 mg, 0.18 mmol) was added and the resulting solution was stirred at room temperature for 10 min. Then MeI (0.015 mL, 0.25 mmol) was added and the reaction mixture was stirred for 15 h at room temperature. The reaction mixture was quenched with saturated NaCl aqueous solution (10 mL) and extracted with EtOAc (3×10 mL) and CH2Cl2 (2×10 mL), The combined organic phases were dried over anhydrous Na2SO4, filtered and concentrated. The crude product thus obtained was chromatographed over silica gel using MeOH/CH2Cl2 mixtures of increasing polarity as eluent, to afford 50 mg of the desired compound (quantitative yield).

Provenance & Evidence