反应详情

4-Iodo acetophenone (10.00 g, 40.64 mmol), PdCl2(dppf).CH2Cl2 (1.00 g, 1.22 mmol) dry dioxane (160 mL) and Et3N (17.0 mL, 121.96 mmol) were combined in a dry flask which had been purged with N2 several times. Pinacol borane (8.80 mL, 60.96 mmol) was added and the reaction mixture was heated at reflux for 4 h then cooled to ambient temperature, poured into Diethyl ether (250 mL) and extracted with H2O and washed with brine. The Diethyl ether was dried (MgSO4), filtered and the filtrate concentrated in vacuo. Purification by gradient chromatography on silica (hexane, 5% EtOAc/hexane) followed by recrystallization (hexane) gave 6.4 g (64%) of the intermediate title compound as a white powder.

1. customwhich had been purged with N2 several times
2. temperaturethe reaction mixture was heated
3. temperatureat reflux for 4 h
4. extractionextracted with H2O
5. washwashed with brine
6. dry with materialThe Diethyl ether was dried (MgSO4)
7. filtrationfiltered
8. concentrationthe filtrate concentrated in vacuo
9. customPurification by gradient chromatography on silica (hexane, 5% EtOAc/hexane)
10. customfollowed by recrystallization (hexane)