反应详情

温度

-30 °C

To a stirred solution of Intermediate 13 (5.1 g) and nickel chloride (12.8 g) in methanol (40 ml) at −30° C., was added sodium borohydride (10.2 g). The reaction was stirred at −30° C. for 30 min, before being stirred at room temperature for 16 h. The solvent was removed in vacuo, and the black slurry was dissolved in aqueous hydrochloric acid (2M, 300 ml), and washed with ethyl acetate (3×200 ml). The aqueous layer was then basified to pH 10 using solid sodium hydroxide, and EDTA added until the solution stayed blue. The aqueous was then extracted with ethyl acetate (3×200 ml), the combined organic extracts dried over magnesium sulphate (4 g), and the solvent removed in vacuo to yield the title compound as a white oily solid (3.2 g).

1. stirringbefore being stirred at room temperature for 16 h
2. customThe solvent was removed in vacuo
3. dissolutionthe black slurry was dissolved in aqueous hydrochloric acid (2M, 300 ml)
4. washwashed with ethyl acetate (3×200 ml)
5. additionadded until the solution
6. extractionThe aqueous was then extracted with ethyl acetate (3×200 ml)
7. dry with materialthe combined organic extracts dried over magnesium sulphate (4 g)
8. customthe solvent removed in vacuo