反应详情

To the solution of the alcohol from EXAMPLE 123 (0.050 g, 0.14 mmol) in dry dichloromethane (3 mL) was added 1,1′-carbonyldiimidazole (0.023 g, 0.14 mmol). The reaction solution was stirred at room temperature for one hour before the methylamine was added. The reaction was then stirred at the same temperature for overnight. The reaction was quenched with 10% HCl aqueous, and extracted with dichloromethane (3 times). The combined organic layer was washed with brine, and dried over anhydrous sodium sulfate. The product was purified via a column chromatography on silica gel. The carbamate was obtained as a white solid, 0.0565 g, 97% yield.

1. additionwas added
2. customThe reaction was quenched with 10% HCl aqueous
3. extractionextracted with dichloromethane (3 times)
4. washThe combined organic layer was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. customThe product was purified via a column chromatography on silica gel