反应详情

温度

100 °C

7 equivalents of LiCl, and then 0.03 equivalents of Pd(PPh3)4 are added, under a stream of argon, to a solution of 52.3 mmol of the product of Preparation 1 and 1.2 equivalents of the product obtained in Step B in 800 ml of dioxane. The reaction mixture is heated to 100° C. and 0.03 equivalent of Pd(PPh3)4 is added in succession, after reaction for 12 hours, 24 hours and 48 hours, and the reaction mixture is maintained at 100° C. for an additional 24 hours. After cooling, filtration over Celite and concentration under reduced pressure, chromatography of the residue on silica gel (dichloromethane/ethanol: 97/3) enables the expected product to be isolated; the product is then crystallised in pentane.

1. customafter reaction for 12 hours
2. temperature24 hours and 48 hours, and the reaction mixture is maintained at 100° C. for an additional 24 hours
3. temperatureAfter cooling
4. filtrationfiltration
5. concentrationover Celite and concentration under reduced pressure, chromatography of the residue on silica gel (dichloromethane/ethanol: 97/3)
6. customto be isolated
7. customthe product is then crystallised in pentane