Phosphorus oxychloride → HCID 86664778, compound

Participants

Reaction Steps

Di-tert-butyl 5-(7-hydroxypyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1,2-dicarboxylate (16.7 mmol, 7.0 g), N,N′-diisopropylethylamine (51.9 mmol, 9.0 ml) and POCl3 (80 mL) were mixed and stirred at room temperature for 18 hours. The solution is concentrated in vacuo and cooled to 0° C. in an ice bath. The reaction is then quenched with sat. NaHCO3(aq) and extracted with DCM (100 mL×3). The combined organics are dried with Na2SO4 and the solvent removed in vacuo. LC-MS: 437 [M+H]. The resulting oil was used in the next step without further purification.

Provenance & Evidence