Thionyl Chloride → HCID 13427179, compound

Participants

Reaction Conditions

Reaction Steps

The acylhydrazine 12 (23.4 g, 75.0 mmol) was added to SOCl2 (200 ml) at 0° C. The reaction was warmed to 60° C. and complete (by TLC) after 3 hours. SOCl2 was removed under reduced pressure. The solid residue was dissolved in EtOAc, washed once with 10% aqueous NaOH and brine. The organic layer was dried over MgSO4, and the solvent was removed under reduced pressure. The crude solid was recrystallized from Et2O to afford 10 (13.0 g, 64.6%), m.p. 81.5°-82.5° C.

Provenance & Evidence