Phosphorus oxychloride → HCID 57438671, compound

Participants

Reaction Conditions

Reaction Steps

Phosphoryl trichloride (4.2 mL, 45 mmol) was added in one portion to 1-(4-methylthiophen-3-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (Intermediate BF2) (700 mg, 3.01 mmol). The resulting suspension was heated to 100° C. to give a solution and stirred for 2 hours. The mixture was evaporated and ice added to the residue and stirred for 30 minutes. It was then filtered and the solids washed with water (3×10 mL). The crude product was dissolved in ethyl acetate (40 mL), dried with MgSO4, filtered and evaporated to give the product (700 mg, 93%).

Provenance & Evidence