反应详情

To a stirred solution of 3-aminopropan-1-ol (2 g, 20 mmol) in DCM (10 mL), imidazole (79 mmol, 3 equiv.) was added and stirred at room temperature for 10 min. Reaction mixture was cooled to 0° C., t-butyl dimethyl silyl chloride (30 mmol, 1.2 equiv.) was added in portions and stirred the reaction mixture overnight at room temperature. Diluted the reaction mixture using DCM, the DCM layer was washed with water. The organic layer was collected, dried over Na2SO4, filtered and concentrated. ELSD method LC/MS: Retention time: 1.5 min; (ES-API), m/z 189.7 (M+H).

1. customReaction mixture
2. temperaturewas cooled to 0° C.
3. stirringstirred the reaction mixture overnight at room temperature
4. additionDiluted the reaction mixture
5. washthe DCM layer was washed with water
6. customThe organic layer was collected
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated