1,3-Dichloropropane → HCID 21389473, compound

Participants

Reaction Steps

The compound of 4-phenoxyphenol (81.03 g, 435.5 mmol) was dissolved in 810 ml MEK at ambient temperature under Nitrogen. Powdered potassium carbonate (577.16 g, 4,176.27 mmol) was added followed by 1,3-dichloropropane (300.00 g, 2,655.1 mmol), and the resulting solution was heated to reflux for 15.5 hours. The solution was cooled to room temperature, filtered and washed with 750 ml MEK. The filtrate was concentrated under vacuum to give a crude orange liquid. The crude liquid was dissolved in 260 ml absolute MeOH at ambient temperature and stirred 5 minutes, which was then cooled in an ice/acetone/water bath for 1.5 hours. White precipitate was filtered off and washed with 480 ml cold absolute MeOH. The white solid was collected and dried under vacuum at 30° C. for 16 hours to afford about 81.87 g of compound (a).

Provenance & Evidence