反应详情

温度

0 °C

To a stirred suspension LiAlH4 (0.77 g, 20.4 mmol) in THF (120 mL) was added a solution of 1,1-dimethylethyl[(1R)-1-methyl-2-phenylethyl]carbamate (2.4 g, 10.2 mmol) in THF (30.0 ml) dropwise at 0° C., and then the reaction mixture was heated at reflux for 2 hours. The mixture was cooled to 0° C., and quenched by addition of ice (1.0 g), then 15% aqueous sodium hydroxide (1.0 mL) followed by water (0.5 mL). The lithium salts were collected by filtration and washed with Et2O (200 mL). The filtrate was dried (Na2SO4), filtered and concentrated. The resulting residue was distilled at reduced pressure to afford the title compound (1.6 g) as a light yellow oil. LC-MS (ES) m/z=150 [M+H]+.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 2 hours
3. customquenched by addition of ice (1.0 g)
4. filtrationThe lithium salts were collected by filtration
5. washwashed with Et2O (200 mL)
6. dry with materialThe filtrate was dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. distillationThe resulting residue was distilled at reduced pressure