Ammonia → HCID 66574956, compound

Participants

Reaction Steps

4 ml of phosphoryl chloride were added to 263 mg (0.571 mmol) of the compound from Example 16A, and the mixture was stirred at RT overnight. The reaction mixture was dissolved in 38 ml of acetonitrile and, with ice-cooling, stirred into 24 ml of concentrated aqueous ammonia solution (33% strength). The mixture was stirred at RT for 2 days. The reaction mixture was then concentrated. The residue was taken up in water and ethanol and stirred at RT for 1 h. The precipitate formed was filtered off with suction and washed with water and ethanol. This residue was purified by preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). This gave 119 mg of the title compound (49% of theory).

Provenance & Evidence