Methyl Isocyanate → 1-(1-Bromo-3-isopropyl-4-oxo-3,4-dihydro-phthalazin-6-yl)-3-methyl-urea

Participants

Reaction Steps

7-Amino-2-Isopropyl-4-bromo-2H-phthalazin-1-one (0.5 g, 1.77 mmol) was dissolved in tetrahydrofuran (THF) (5 ml). To this was added NaH (60%, 0.14 g, 3.54 mmol) as a suspension in THF (2 ml) and the reaction mixture was stirred for 5 minutes. After this time methyl isocyanate (0.2 g, 3.55 mmol) was added in one portion and the reaction mixture was stirred at room temperature for a further 48 hours. After this time, the reaction mixture was partitioned between ethyl acetate (50 ml) and water (50 ml), the organic layer was separated, dried (MgSO4), filtered and concentrated under vacuum to give the title compound (0.47 g, 78% yield) as a light brown solid.

Provenance & Evidence