反应详情

A solution of 4-(3-{3-[(2-chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (475 mg, 0.67 mmol) in a 1:1 mixture of 3M HCl (aq.) and methanol (30 mL total) was stirred at room temperature for 18 hours. The mixture was concentrated in vacuo, and the crude material was dissolved in EtOAc. The EtOAc solution was washed with saturated aqueous sodium bicarbonate solution (3×) and brine (1×), dried over sodium sulfate, and filtered. The EtOAc extracts were concentrated and the crude piperazine was treated with 1 M HCl (Et2O) to afford the title compound as a solid, 415 mg (100%). MS(ES) m/e 608.4 (M+).

1. concentrationThe mixture was concentrated in vacuo
2. dissolutionthe crude material was dissolved in EtOAc
3. washThe EtOAc solution was washed with saturated aqueous sodium bicarbonate solution (3×) and brine (1×)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationThe EtOAc extracts were concentrated
7. additionthe crude piperazine was treated with 1 M HCl (Et2O)