反应详情

To a solution of crude 61I (˜1.81 mmol) in CH2Cl2 (10 mL) was added i-Pr2NEt (2 mL) followed by 20% phosgene in toluene (2.5 mL) dropwise. The reaction was stirred at rt overnight. Reaction was extracted with EtOAc (50 mL) which was washed twice with 1N HCl and then saturated NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated. Purification by flash chromatography (silica gel, 0 to 10% EtOAc in hexane) provided the title compound (369 mg): MS (ES) m/z 420.23 [M+H]+

1. customReaction
2. extractionwas extracted with EtOAc (50 mL) which
3. washwas washed twice with 1N HCl
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by flash chromatography (silica gel, 0 to 10% EtOAc in hexane)