Phosphorus oxychloride → HCID 59312985, compound

Participants

Reaction Conditions

Reaction Steps

575 mg (1.3 mmol) of 3,8-dibromo-7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidin-5-ol (Example 123A) are introduced into phosphoryl chloride (5 ml), 900 mg (4 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 12 h. The reaction mixture is slowly poured, while stirring vigorously, into saturated sodium bicarbonate solution, and solid sodium bicarbonate (approx. 3 g) is added until a pH of 10 is reached. The mixture is stirred for 10 min, ethyl acetate (100 ml) is added and shaken, and the organic phase is separated off, washed with water and dried over magnesium sulphate and concentrated in a rotary evaporator. The residue is purified by silica gel chromatography (cyclohexane/ethyl acetate 10:1). 480 mg (80% of theory) of the product are obtained.

Provenance & Evidence