反应详情

温度

70 °C

Borane (1M solution in THF, 10 mL, 10 mmol) was added slowly dropwise to a solution of 16C (0.98 g, 4.37 mmol) in THF (60 mL) at 0° C. The reaction mixture was then heated to 70° C. overnight. The reaction mixture was cooled in an ice bath and quenched by cautious addition of hydrochloric acid (2N, 12 mL, 24 mmol). The reaction mixture was refluxed for 2 h and then concentrated almost to dryness in vacuo. The residue was coevaporated with methanol (3×), diluted with ethyl acetate and sodium hydroxide solution (2N). The aqueous layer was extracted with ethyl acetate (3×), dried (MgSO4), and concentrated in vacuo to give 16D (1.03 g, 100%) as a clear oil. MS (ESI) m/z 211.1 (M+H)+.

1. temperatureThe reaction mixture was cooled in an ice bath
2. temperatureThe reaction mixture was refluxed for 2 h
3. concentrationconcentrated almost to dryness in vacuo
4. additiondiluted with ethyl acetate and sodium hydroxide solution (2N)
5. extractionThe aqueous layer was extracted with ethyl acetate (3×)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo