反应详情

A mixture of 1-{4-[1-(tert-butoxycarbonyl)-4-hydroxypiperidin-4-yl]phenyl}cyclopropanecarboxylic acid (300 mg, prepared as described in example 210, steps 1 & 2) and trifluoroacetic acid 2 mL was stirred at rt for 5 h. The reaction mixture was then concentrated. The crude product was dissolved in tetrahydrofuran (4 mL, 0.05 mol) and to this was added di-tert-butyldicarbonate (333 mg, 0.00152 mol) and N,N-diisopropylethylamine (6.0×10−2 μL, 0.0035 mol). The mixture was stirred at rt for 5 h and then diluted with AcOEt, washed with saturated NaHCO3 aqueous solution and 1M HCl successively, dried with MgSO4, and concentrated in-vacuo to afford the desired product.

1. concentrationThe reaction mixture was then concentrated
2. stirringThe mixture was stirred at rt for 5 h
3. washwashed with saturated NaHCO3 aqueous solution and 1M HCl successively
4. dry with materialdried with MgSO4
5. concentrationconcentrated in-vacuo