反应详情

温度

80 °C

In a dry 10 mL Schlenk-tube, which has been flooded with argon, [Mo(≡N)(OSiPh3)3(phen)].0.5 toluene (50.0 μmol, 58.1 mg) and MnCl2 (50.0 μmol, 6.3 mg) were suspended in 2.5 mL of toluene. After addition of 1-phenyl-1-propine (500 μmol, 58.1 mg), the reaction solution was stirred for 24 h at 80° C. and was filtered after cooling over a short silica gel column. The filtrate was concentrated and the residue was purified by column chromatography (hexane). 41.6 mg of tolane (93%) were isolated as white solid, the spectroscopic and analytical data of which were identical to those of a commercial sample. M.p.=59-61° C.

1. filtrationwas filtered
2. temperatureafter cooling over a short silica gel column
3. concentrationThe filtrate was concentrated
4. customthe residue was purified by column chromatography (hexane)