反应详情

TFAA (0.20 ml, 1.4 mmol) was added to a suspension of Compound 215-11-COOH (144 mg, 0.403 mmol) in toluene (5 ml) at 0° C., and the mixture was allowed to warm to room temperature with stirring for 30 minutes. After checking for complete dissolution of the raw material, the mixture was again cooled to 0° C. tBuOH (0.40 ml, 4.2 mmol) was added to the cooled mixture, which was allowed to warm to room temperature with stirring for 15 hours. A saturated aqueous NaHCO3 solution was added to the reaction solution, which was extracted with EtOAc twice after stirring for 5 minutes. The combined organic layer was washed with a saturated aqueous NaCl solution, and was dried over anhydrous Na2SO4. After evaporation of the solvent, the residue was purified by column chromatography on silica gel (Hexane:EtOAc=7:1 to 4:1) followed by PTLC (Hexane:EtOAc=7:1) to yield the target product (28 mg, 17%).

1. additionwas added to the cooled mixture, which
2. temperatureto warm to room temperature
3. stirringwith stirring for 15 hours
4. extractionwas extracted with EtOAc twice
5. stirringafter stirring for 5 minutes
6. washThe combined organic layer was washed with a saturated aqueous NaCl solution
7. dry with materialwas dried over anhydrous Na2SO4
8. customAfter evaporation of the solvent
9. customthe residue was purified by column chromatography on silica gel (Hexane:EtOAc=7:1 to 4:1)