Pyridine → HCID 11635478, compound

Participants

Reaction Steps

Compound 101 (57 mg, 1.5 mmol)) was dried by co-evaporation with dry pyridine (2×5 mL) and toluene (2×5 mL) and suspended in trimethylphosphate (5 mL). Phosphoro oxychloride (1.2 eq.) was added and reaction mixture kept for 2 h at 5° C. Tributylammonium pyrophosphate (1 mL of 2N solution in DMF) was added and the mixture was left overnight at 5° C. Reaction was quenched with Et3NHCO3 buffer and separated by RP-HPLC from 0 to 100% B, buffer A—water, buffer B—CH3CN. The major peak was collected, concentrated and repurified by RP-HPLC from 0 to 60% B. Buffers were as mentioned above. The major peak was collected and lyophilized;

Provenance & Evidence