反应详情

To the solution of compound 1 (10 g, 54.6 mmol) and triethylamine (15 mL, 106 mmol) in 200 mL of dichloromethane was added benzyl chloroformate (7.24 mL, 51.5 mmol, diluted in 100 mL of dichloromethane) dropwise at 0° C. After the addition, the solution was stirred at r.t. for one hour. The solid was removed by filtration. The solution was extracted with 100 mL of 0.1 M HCl and 100 mL of sat. sodium carbonate, and dried over anhydrous sodium sulfate. Removal of solvent provided a white solid that was stirred in 200 mL of THF/hexane (1:20) for three hours. The solid was collected by filtration to give 14.2 g of the target compound in 87% yield.

1. additionAfter the addition
2. customThe solid was removed by filtration
3. extractionThe solution was extracted with 100 mL of 0.1 M HCl and 100 mL of sat. sodium carbonate
4. dry with materialdried over anhydrous sodium sulfate
5. customRemoval of solvent
6. customprovided a white solid
7. filtrationThe solid was collected by filtration