反应详情

温度

120 °C

N-{2-tert-Butyl-1′-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}acetamide (500 mg, 1.37 mmol) was dissolved in 10 mL of 1:1/EtOH:2M HCl. The solution was divided into two sealed tubes (5 mL/tube). Each tube was heated at 120° C. in a Personal Chemistry microwaves instrument for 1 h. The fractions were pooled and the solvent was evaporated. The residue was diluted with 2M NaOH and extracted (3×) with EtOAc. The organic phase washed with saturated aqueous NaCl solution and dried over anhydrous Na2SO4. The solvent was evaporated. Yield: 440 mg (99%). 1H NMR (400 MHz, CHLOROFORM-D) δ 1.40-1.52 (m, 2H), 1.52-1.54 (m, 9H), 1.56-1.66 (m, 4H), 1.68-1.75 (m, 2H), 2.07-2.17 (m, 3H), 4.14 (d, J=7.62 Hz, 2H), 6.65 (dd, J=8.50, 2.25 Hz, 1H), 7.04-7.09 (m, 2H).

1. customthe solvent was evaporated
2. additionThe residue was diluted with 2M NaOH
3. extractionextracted (3×) with EtOAc
4. washThe organic phase washed with saturated aqueous NaCl solution
5. dry with materialdried over anhydrous Na2SO4
6. customThe solvent was evaporated