反应详情

To a solution of (R)-2-Amino-1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methylbutan-1-one hydrochloride (250 mg, 0.75 mmol) in DCM (2 mL) was added DIEA (175 μL, 1 mmol) followed by the dropwise addition of benzoylisothiocyanate (106 μL, 0.78 mmol). The reaction was stirred for 2 h at rt., acidified with 1 N aqueous HCl solution to pH 3 and then extracted with Et2O (3×10 mL). The extracts were combined, washed sequentially with sat. aqueous NaHCO3 solution (1×10 mL) and sat. aqueous NaCl solution (1×10 mL), dried (MgSO4), and the solvent removed to give (R)—N-(1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methyl-1-oxobutan-2-ylcarbamothioyl)benzamide (m/z, 458, M+1) as an oil (300 mg) in greater than 90% HPLC purity.

1. extractionextracted with Et2O (3×10 mL)
2. washwashed sequentially with sat. aqueous NaHCO3 solution (1×10 mL) and sat. aqueous NaCl solution (1×10 mL)
3. dry with materialdried (MgSO4)
4. customthe solvent removed