反应详情

温度

80 °C

A mixture of [3-(tert-butyl-dimethyl-silanyloxymethyl)-4-chloro-benzyl]-carbamic acid methyl ester (5.39 g, 15.7 mmol) in MeOH (160 mL) and aq. 1M NaOH (80 mL) was heated to 80° C. for 1.5 h. The mixture was allowed to cool to rt, and was partially evaporated under reduced pressure. The aq. residue was extracted with EtOAc (3×). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Drying the residue under high vacuum yielded the crude title compound (3.53 g, 98%) that was used further without purification. LC-MS: tR=0.72 min; ES+: 230.25.

1. temperatureto cool to rt
2. customwas partially evaporated under reduced pressure
3. extractionThe aq. residue was extracted with EtOAc (3×)
4. dry with materialextracts were dried over MgSO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure
7. customDrying the residue under high vacuum