反应详情

tert-Butyl carbamate 199 (224 mg, 0.30 mmol) is deprotected using Method F. On removal of the solvents in vacuo, the residue is suspended in aqueous NaHCO3 (20 mL) and extracted into DCM (3×20 mL). The combined DCM phases are washed with water (2×20 μL) and brine (20 mL) then dried (Na2SO4) and reduced in vacuo. The free base thus obtained is converted to the HCl salt by Method H. The isolated salt is then dissolved in the minimum amount of DCM and added dropwise to cold (0° C.) TBME (25 mL). The resultant pale yellow precipitate is isolated by filtration, washed with TBME (10 mL) and diethyl ether (10 mL) and dried to afford the title compound.

1. customOn removal of the solvents in vacuo
2. extractionextracted into DCM (3×20 mL)
3. washThe combined DCM phases are washed with water (2×20 μL) and brine (20 mL)
4. dry with materialthen dried (Na2SO4)
5. customThe free base thus obtained
6. customThe resultant pale yellow precipitate is isolated by filtration
7. washwashed with TBME (10 mL) and diethyl ether (10 mL)
8. customdried