反应详情

Trifluoroacetic acid (8.6 mL, 111 mmol) was added to a solution of compound 9 (5.56 g, 15 mmol) in dichloromethane (50 mL). The reaction mass was stirred at room temperature for 24 h and evaporated in vacuo. The residue was diluted with water (50 mL), and the obtained solution was extracted with CH2Cl2. The organic layer was discarded. The aqueous one was alkalized with 10 N NaOH to pH 12 and extracted with CHCl3 (3×100 mL). The combined extracts were dried and evaporated to afford the title compound (3 g, 74%) as a yellow oil. LCMS-data: M+H 275.2, 276.2 (calc. 274.4). 1H NMR-data (DMSO-d6): 7.16 (d, 2H, Ph, J=8.6); 6.72 (d, 2H, Ph, J=8.6); 4.65-4.78 (m, 1H); 3.46 (s, 2H, CH2); 2.56 (d, 2H, CH2, J=7.6); 2.34-2.41 (m, 4H); 2.28 (s, 3H, NCH3); 2.00-2.30 (m, 5H); 1.60-1.71 (m, 4H).

1. customevaporated in vacuo
2. additionThe residue was diluted with water (50 mL)
3. extractionthe obtained solution was extracted with CH2Cl2
4. extractionextracted with CHCl3 (3×100 mL)
5. customThe combined extracts were dried
6. customevaporated