反应详情

To a mixture of the product of step B (1.5 g, 2.9 mmol) and NMM (590 mg, 5.83 mmol) in DME (15 mL) was added isobutyl carbonochloridate (793 mg, 5.83 mmol) dropwise at 0° C. After stirring for 30 min. NaBH4 was added to the mixture at 0° C. The resulting mixture was stirred at room temperature for another 1 h, and then quenched with saturated ammonium chloride solution (10 mL), extracted with ethyl acetate. The organic layers were washed with brine (10 mL), dried over sodium sulfate, filtered and evaporated. The residue was purified by silica gel chromatography (PE:EA=3:1) to afford the title compound as colorless oil. LC/MS m/z=501.2[M+H]+.

1. stirringThe resulting mixture was stirred at room temperature for another 1 h
2. customquenched with saturated ammonium chloride solution (10 mL)
3. extractionextracted with ethyl acetate
4. washThe organic layers were washed with brine (10 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by silica gel chromatography (PE:EA=3:1)