实验操作Compound 26 was charged to a reactor and 2-MeTHF (5V) added. The mixture was headed to 60- 70°C. In a separate vessel, 2-MeTHF (4V), potassium tertbutoxide (KOtBu) (0.25 equiv.), and HPPh2 (0.4 equiv) were mixed and then added to the substrate-containing vessel. The mixture was stirred at 60-70°C for 4 hours. More KPPh2 was prepared in the same quantity and the sequence repeated twice more (three total additions of equal amounts). The mixture was heated at 65-75°C for 16 hours and the temperature adjusted to 10-20°C.
2N HCl (2 equiv.) was added and the mixture stirred for 20 hours, maintaining the temperature. Aqueous K2CO3 (0.5 equiv.) was charged, the mixture stirred, and layers separated (the aqueous layers were maintained at a temperature of 10-20°C. The retained aqueous layer was washed five times with DCM. The combined organics were concentrated to 2-3V and solvent swapped into MTBE with three cycles. The mixture was heated to 35-45°C then cooled to 0-10°C and stirred at that temperature for 10 hours. The solids were isolated by filtration, washed with MTBE, and dried under vacuum. Average yield over 2 batches: 64.0%
