反应详情

A solution of (0.1 mmol) of 10, (0.12 mmol) of 4, 14 mg (0.13 mmol) of neopentyl glycol, 95 mg (0.3 mmol) of Ba(OH)2.8H2O, 80 μl (6.08 mmol, 5 mol %) of a 76 mM acetone solution of Pd(OAc)2 in 2 ml of 95% i-PrOH is stirred at 80° C. for 12 hours. The solvent is subsequently removed under reduced pressure. 2 ml of 2 M HCl are added to the residue, and the mixture is extracted with dichloromethane (3×2 ml). The combined organic phases are dried over MgSO4 and filtered through SiO2. The solvent is removed under reduced pressure, and the residue is purified by recrystallisation twice from nonane (yield: 60%).

1. customThe solvent is subsequently removed under reduced pressure
2. addition2 ml of 2 M HCl are added to the residue
3. extractionthe mixture is extracted with dichloromethane (3×2 ml)
4. dry with materialThe combined organic phases are dried over MgSO4
5. filtrationfiltered through SiO2
6. customThe solvent is removed under reduced pressure