反应详情

温度

100 °C

A flame-dried Schlenk tube containing a Teflon coated stir bar was charged with Pd(OAc)2 (20 mg, 0.088 mmol), (2-dicyclohexylphosphino)-2′,4′,6′-triisopropyl biphenyl (105 mg, 0.22 mmol), 1,3-cyclopentanedione (65 mg, 0.66 mmol), toluene-4-sulfonic acid 6-(3-adamantan-1-yl-4-methoxyphenyl)-naphthalen-2-yl ester (238 mg, 0.44 mmol) and finely ground K3PO4 (233 mg, 1.1 mmol). The tube was capped with a septum, evacuated and backfilled with nitrogen three times, 2 mL of dry dioxane was injected and the mixture was heated to 100° C. for 3 h. The mixture was then cooled, diluted with EtOAc, washed with 1N HCl, dried over Na2SO4 and filtered. The filtrate was concentrated and purified by flash chromatography using MeOH—CH2Cl2.

1. additionA flame-dried Schlenk tube containing a Teflon coated stir bar
2. customThe tube was capped with a septum
3. customevacuated
4. temperatureThe mixture was then cooled
5. additiondiluted with EtOAc
6. washwashed with 1N HCl
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationThe filtrate was concentrated
10. custompurified by flash chromatography