反应详情

A tube was charged with 66.15D (213 mg, 552 μmol), N-ethyl-N-isopropylpropan-2-amine (143 mg, 1103 μmol) and toluene, evacuated and back-filled with nitrogen three times. Pd2(dba)3, 4,5-bis(diphenylphosphino)-9,9-dimethyl-9H-xanthene (31.9 mg, 55.2 μmol) and propane-2-thiol (63.0 mg, 827 μmol) were added to the mixture and then the mixture was degassed three times. The suspension was refluxed overnight, filtered, and concentrated to give a residue which was purified by silica gel chromatography to give 69.24A as a pale yellow solid (164 mg, 89%). MS ESI m/e: 335.2 (M+1)+.

1. customevacuated
2. additionback-filled with nitrogen three times
3. customthe mixture was degassed three times
4. temperatureThe suspension was refluxed overnight
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a residue which
8. customwas purified by silica gel chromatography