反应详情

To a 1M Et2O solution of LiAlH4 (200 mL, 200 mmol) at 0° C., slowly add the product of Step 2 (14.35 g, 49.1 mmol) dissolved in tetrahydrofuran (THF) (100 mL). Allow the reaction mixture to warm to room temperature and stir for 45 min. After recooling to 0° C., quench the excess LiAlH4 by the careful addition of aqueous saturated Na2SO4 (20 mL). Dry the solution with Na2SO4 and filter. Wash the lithium salts with Et2O (3×300 mL). Concentrate the combined filtrates to give 8.65 g of 4-amino-3-(3,4-dichlorophenyl)-butanol as a white solid (36.9 mmol, 75%).

1. customAfter recooling to 0° C.
2. customquench the excess LiAlH4
3. additionby the careful addition of aqueous saturated Na2SO4 (20 mL)
4. dry with materialDry the solution with Na2SO4
5. filtrationfilter
6. washWash the lithium salts with Et2O (3×300 mL)
7. concentrationConcentrate the combined filtrates