反应详情

温度

0 °C

The compound (3.69 mmol) obtained in Step 5 and NaHCO3 (11.07 mmol) were distilled with tetrahydrofuran (40 mL) and distilled water (6 mL), and acryloyl chloride (3.69 mmol) was added thereto slowly at 0° C. with stirring for 15 min. After the reaction was complete, the reaction mixture was distilled with dichloromethane and then washed with sat. NaHCO3 aqueous solution. The organic layer was dried with anhydrous sodium sulfate and then filtered and distilled under a reduced pressure, and the residue was separated by column chromatography (chloroform:methanol=20:1 (volume ratio)) to obtain the title compound (yield: 68.2%).

1. additionwas added
2. distillationthe reaction mixture was distilled with dichloromethane
3. washwashed with sat. NaHCO3 aqueous solution
4. dry with materialThe organic layer was dried with anhydrous sodium sulfate
5. filtrationfiltered
6. distillationdistilled under a reduced pressure
7. customthe residue was separated by column chromatography (chloroform:methanol=20:1 (volume ratio))