Diisopropylethylamine → HCID 178443925, compound

Participants

Reaction Steps

To a solution of (15) (0.131 g, 0.216 mmol) stirring at room temperature under argon in anhydrous DMF (2.0 ml), 1-H-pyrazole-1-carboxamidine•HCl (32 mg, 0.216 mmol) was added followed by diisopropylethylamine (28 ml, 0.216 mmol). The reaction mixture was stripped slightly on a rotovap then rotated overnight without vacuum at room temperature. After removing DMF in vacuo the reaction residue was dissolved in dichloromethane and applied to a flash silica gel column. An isocratic system of 20% MeOH/dichloromethane, 2% NH4OH followed by treatment with Dowex OH− (300 mg) in MeOH gave 80 mg of desired product (yield, 57%). 31P NMR (s, 31.99 ppm), mass spec. calcd=648.91, Found=649.48.

Provenance & Evidence