Hydrochloric Acid → HCID 54478463, compound

Participants

Reaction Steps

To a suspension of 1-methyl-2-nitroisourea (1.5 g) in water (15 ml), methylamine hydrochloride (0.9 g) was added (pH: 3.3). An aqueous sodium hydroxide (1%) was gradually added to maintain the pH of the suspension at 8 at room temperature. After the suspension was stirred for 3 hours at room temperature while maintaining the pH thereof to 8, an aqueous hydrochloric acid (4 M) was added, and then the solution was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, and it was then concentrated under reduced pressure. The residual oil was purified by silica gel column chromatography (hexane/ethyl acetate: 2/1) and then recrystallized (ethyl acetate-hexane), to obtain the desired compound (1.0 g) as colorless crystals.

Provenance & Evidence