Biphenyl → HCID 11129642, compound

Participants

Reaction Steps

To a 100 ml, three-necked, frame dried, round bottom flask equipped with a magnetic stirrer, a reflux condenser, and a dropping funnel, aluminum chloride 1.43 g (10.7 mmol) and biphenyl 16.5 g (107 mmol) were placed under dry nitrogen atmospheric pressure. After (dichloromethyl)methyldichlorosilane 7.50 ml (53.5 mmol) was added to the solution, the reaction mixture was heated for 2.5 hrs. at 120° C. The aluminum chloride catalyst was quenched with POCl3 1.04 ml (11.2 mmol) and then stirred for another 1 hr. to complete the deactivation. Freshly distilled hexane (100 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic solution. After hexane was distilled, the reaction products were vacuum distilled at 0.2 torr to give 8.79 g of 9-(methyldichlorosilyl)fluorene (bp; 115°-120° C./0.2 torr, yield; 59%).

Provenance & Evidence