反应详情

温度

0 °C

To a suspension of LiAlH4 (8.18 g; 215.6 mmol) in THF (100 mL), was added dropwise a solution of 2-azido-1-(4-benzyloxy-phenyl)-ethanone (23.05 g; 86.2 mmol) in THF (200 mL), at 0° C. The mixture was stirred at 0° C. for 20 min. and subsequently 2 hours at RT. Thereafter, water (50 mL), and 2M aqueous NaOH-solution (150 mL) were added consecutively. The formed precipitate was removed by filtration over kieselguhr, and washed with MeOH. The filtrate was concentrated in vacuo and the remaining aqueous layer was extracted with CH2Cl2. The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo to afford 2-amino-1-(4-benzyloxy-phenyl)ethanol (20.10 g)

1. customat 0° C
2. customThe formed precipitate was removed by filtration over kieselguhr
3. washwashed with MeOH
4. concentrationThe filtrate was concentrated in vacuo
5. extractionthe remaining aqueous layer was extracted with CH2Cl2
6. dry with materialThe combined organic layers were dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo