反应详情

LiAlH4 (2.7 g, 0.07 mol) was added to a solution of intermediate 7, N-Benzyl-3-oxocyclobutanecarboxamide (7.12 g, 0.035 mol) in absolute THF (100 mL) under stirring in argon. The mixture was refluxed under stirring for 2 h and cooled. Then 10 N NaOH (2 mL) and water (1 mL) were added. The organic layer was decanted, and the aqueous one was extracted with THF (2×50 mL). The organic layers were evaporated to afford the title compound (3.9 g, 58%) as a colorless oil. 1H NMR-data (DMSO-d6): 7.00-7.49 (m, 6H, NH, Ph); 4.80 (br.s, 1H, OH); 3.81-3.95 (m, 1H); 3.67 (s, 2H, CH2); 2.48 (d, 2H, CH2, J=6.8 Hz); 2.19-2.30 (m, 2H); 1.70-1.84 (m, 1H); 1.35-1.50 (m, 2H).

1. temperatureThe mixture was refluxed
2. stirringunder stirring for 2 h
3. temperaturecooled
4. customThe organic layer was decanted
5. extractionthe aqueous one was extracted with THF (2×50 mL)
6. customThe organic layers were evaporated