Hydrochloric Acid → HCID 67324574, compound

Participants

Reaction Steps

To a solution of 1,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate (1.5 g, 7.49 mmol, supplier Aldrich) and N,N-diisopropylethylamine (1.962 mL, 11.23 mmol) in dry DCM (20 mL) was added 4-[(difluoromethyl)oxy]benzenesulfonyl chloride (1.253 mL, 7.86 mmol, supplier Aldrich) dropwise. The solution was stirred at room temperature for 4 h and then left to stand for 16 h. The solution was washed with aqueous sodium bicarbonate (20 mL), 0.5 M HCl (20 mL) and brine (20 mL) before the organic phase was isolated by phase separator. To the solution was added hydrochloric acid (1.872 mL, 7.49 mmol) 4M in dioxane and the reaction stirred at room temperature for 3 h. LCMS showed only partial reaction, so further hydrochloric acid (1.872 mL, 7.49 mmol) 4M in dioxane was added and the reaction stirred for 21 h. The reaction mixture was then concentrated under vacuum to give the title compound (2.448 g) as a pale yellow solid.

Provenance & Evidence