Methyl iodide → HCID 85705623, compound

Participants

Reaction Steps

N-butyloxycarbonylbutylamine (140 mg, 0.80 mmole) was dissolved in DMF (8 ml), and sodium hydride (NaH, 20 mg, 1 eq. wt.) and iodomethane (0.10 ml, 2 eq. wt.) were added thereto. The reaction mixture was stirred for 30 minutes at room temperature and filtered through celite bed and then concentrated under reduced pressure to remove the solvent. The residue was diluted with ethyl acetate, washed with 0.5N aqueous hydrochloric acid solution, dried over anhydrous magnesium sulfate and filtered. The organic layer was concentrated under reduced pressure and dried by means of a vaccum pump to obtain a white solid, which was then dissolved in dichloromethane and cooled down to 0° C. To this mixture was added 1 ml of trifluoroacetic acid (TFA). The reaction solution was stirred for 30 minutes at room temperature, concentrated under reduced pressure and then dried by means of a vaccum pump to obtain the title compound (0.16 g) in a quantitative yield.

Provenance & Evidence