Lithium iodide → HCID 136029315, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of a solution of 2,7-bis(5-methylbenzoxazol-2-yl)-9,9-dipropyl-3-methoxyfluorene] (34.6 g, 0.0638 mol) and 2,4,6-collidine (250 mL) that was prepared under argon by stirring and heating to 95° C. To this solution, dry lithium iodide (14.9 grams, 0.111 mol) was added and the resulting mixture was heated to reflux for 30 minutes and then allowed to cool to room temperature. The reaction was quenched with a mixture of concentrated HCl (167 mL), water (300 mL) and ice (500 g). The product was collected and washed with a minimum of water and methanol to afford upon drying crude product (40 g). Purification by extraction from of acidic alumina (3 cm3) on Ace-Kauffman column with methylcyclohexane gave 2,7-bis(5-methylbenzoxazol-2-yl)-9,9-dipropyl-3-hydroxyfluorene (24.93 g, yield 74%).

Provenance & Evidence