反应详情

温度

-10 °C

To a solution of Intermediate 7A (3.1 g, 10.09 mmol) in EtOH (30 ml) was added calcium chloride (0.336 g, 3.03 mmol). The resulting mixture was cooled to −10° C. and sodium borohydride (0.955 g, 25.2 mmol) was added. The mixture was then allowed to warm to rt and stand at rt. for 1 h. The reaction mixture was diluted with EtOAc and Sat. NaHCO3, extracted with EtOAc (×3). The combined organic layer was dried (MgSO4), concentrated to yield Intermediate 7B (2.68 g, 10.11 mmol, 100% yield) as a white solid. 19F NMR (376 MHz, methanol-d3) δ ppm −98.12 (br. s., 2F). 1H NMR (400 MHz, methanol-d3) δ ppm 2.42 (t, J=4.39 Hz, 6H) 3.92 (t, J=14.06 Hz, 2H) 7.26 (s, 2H).

1. temperatureto warm to rt
2. customstand at rt
3. extractionextracted with EtOAc (×3)
4. dry with materialThe combined organic layer was dried (MgSO4)
5. concentrationconcentrated