Methyl iodide → HCID 68453284, compound

Participants

Reaction Conditions

Reaction Steps

A Grignard reagent was prepared with magnesium (84 mg, 3.5 mmol) and CH3I (0.2 ml, 3.5 mmol) in dry ether (1 ml, distilled over sodium) under N2 atmosphere. (6a) (360 mg, 1 mmol) in ether (0.5 ml) was added to the stirred solution and the ether was distilled. The residue was heated under N2 atmosphere till 210° C. for 45 min. Then the flask was cooled till room temperature and the reaction was quenched with ice water. The aqueous solution was extracted several times with ether. The combined organic extracts were dried on MgSO4 and filtered. Removal of the solvents under reduced pressure afforded a residue that was chromatographed on silica gel (25% Ether/P.E.) to give 132 mg of the pure (11a) (yield 40%).

Provenance & Evidence