反应详情

1,4-Dioxa-8-azaspiro[4,5]decane (653 g, 4.56 mol), 1-(benzyloxy)-4-iodobenzene (1 kg, 3.8 mol), sodium tert-butoxide (511 g, 5.32 mol), Pd(OAc)2 (17 g, 76 mmol) and biphenyl-2-yl(dicyclohexyl) phosphine (54 g, 152 mmol) were mixed, and 1,4-dioxane, this was stirred overnight at 80° C. in a nitrogen atmosphere. The reaction solution was cooled with ice, diluted with ethyl acetate, washed with water and saturated saline in that order, and the organic layer was dried with sodium sulfate. The solvent was evaporated off under reduced pressure, and the resulting residue was purified through silica gel column chromatography (eluate: chloroform/ethyl acetate=10/1), and the resulting crude product was suspended in a mixed solvent of chloroform/hexane and filtered under suction to obtain the entitled compound (910 g, 73%) as a brown solid.

1. temperatureThe reaction solution was cooled with ice
2. washwashed with water and saturated saline in that order
3. dry with materialthe organic layer was dried with sodium sulfate
4. customThe solvent was evaporated off under reduced pressure
5. customthe resulting residue was purified through silica gel column chromatography (eluate: chloroform/ethyl acetate=10/1)
6. filtrationfiltered under suction