反应详情

To an ice-cold solution of (2-chloro-4-iodo-pyridin-3-yl)-methyl-carbamic acid tert-butyl ester (0.97 g, 2.63 mmol) in CH2Cl2 (5 mL) was added TFA (6.00 g, 4.05 mL, 52.6 mmol) and the solution was stirred at room temperature for 1.5 hours before another TFA (6.00 g, 4.05 mL, 52.6 mmol) was added. After stirring at room temperature for 3 hours the clear solution was evaporated. The residue was taken up in saturated aqueous NaHCO3 solution (50 mL) and CH2Cl2 (30 mL) and the layers were separated. The aqueous layer was extracted twice with CH2Cl2 (30 mL each) and the organic layers were washed with brine, dried over MgSO4, filtered and evaporated. Colorless oil (0.61 g; 86%). MS (ESI): m/z=268.93 [M+H]+.

1. additionwas added
2. customwas evaporated
3. customCH2Cl2 (30 mL) and the layers were separated
4. extractionThe aqueous layer was extracted twice with CH2Cl2 (30 mL each)
5. washthe organic layers were washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated