Diethylene Glycol → HCID 22935640, compound

Participants

Reaction Conditions

Reaction Steps

A Dean-Stark trap with reflux condenser was fitted to a 1 liter conical flask, and 2,7-di(1-oxopentyl)fluorene (30.4129 g, 91.0566 mmol), hydrazine monohydrate (44.2 ml) and diethylene glycol (400 ml) were introduced and heated at 130° C. After 2 hours, KOH (20.5628 g) was added and heated at 200° C. After 3 hours, the reaction liquid was returned to room temperature, water was added, and the organic layer was extracted twice with ether. The organic layer was washed with 1N-HCl, saturated sodium bicarbonate solution, water (twice) and a saturated salt solution, and dried using MgSO4. The solution obtained was filtered, and concentrated under reduced pressure to obtain a crude product (27.6591 g, yellow solid). The crude product was purified by silica gel chromatography (hexane) to obtain 2,7-di-n-pentylfluorene (26.2137 g, yellow solid).

Provenance & Evidence