反应详情

温度

100 °C

A 300 ml. stainless steel high pressure reactor was charged, under a nitrogen atmosphere at atmospheric temperature, with a solution of ##STR1## hereinafter referred to as Nb(OC6H3Ph2 --2,6)2 (CH2C6H4 --4Me)3 (2.2 g., 2.5 mmol.) and bis(di-phenylphosphino)methane (25.0 g., 65.1 mmol.) in cyclohexane (55 ml.). The reactor was pressurized with hydrogen (1,200 psi) and heated at 100° C. for four days. During the course of the reaction the pressure dropped requiring the repressurization of the reactor four times. Thereupon, the reactor was cooled and the hydrogen gas vented. The cyclohexane was removed in vacuo and water (30 ml.) was added to the mixture. The mixture was extracted with diethyl ether (200 ml.) which extraction was repeated four times to yield a clear colorless solution. The ether was removed and the resultant solution was recrystallized from hot ethanol (120 ml.).

1. additionstainless steel high pressure reactor was charged, under a nitrogen atmosphere at atmospheric temperature, with a solution of ##STR1##
2. customDuring the course of the reaction the pressure
3. additiondropped
4. temperatureThereupon, the reactor was cooled
5. customThe cyclohexane was removed in vacuo and water (30 ml.)
6. additionwas added to the mixture
7. extractionThe mixture was extracted with diethyl ether (200 ml.) which extraction
8. customto yield a clear colorless solution
9. customThe ether was removed
10. customthe resultant solution was recrystallized from hot ethanol (120 ml.)