反应详情

温度

0 °C

To a mixture of NaBH4 (2.247 g, 59.08 mmol) and LiCl (2.505 g, 59.08 mmol) in EtOH (42 mL), stirring under nitrogen at 0° C., was added (35) (7.659 g, 29.54 mmol) in THF (30 mL) dropwise. This mixture was allowed to warn to room temperature and continued stirring for 48 hours. The precipitate was filtered and washed with ethanol. The washings were concentrated and extracted with EtOAc. The organic layer was then washed with brine and dried over anhydrous Na2SO4. Column chromatography on SiO2 (1:1 EtOAc/Hexanes) was utilized to purify 6.101 g (89%) of the title compound as a white solid.

1. customto warn to room temperature
2. stirringcontinued stirring for 48 hours
3. filtrationThe precipitate was filtered
4. washwashed with ethanol
5. concentrationThe washings were concentrated
6. extractionextracted with EtOAc
7. washThe organic layer was then washed with brine
8. dry with materialdried over anhydrous Na2SO4
9. customto purify 6.101 g (89%) of the title compound as a white solid