1-Naphthol → HCID 35631, compound

Temperature

0 °C

In a 2 l round-bottom flask, 125.0 g of cyanuric chloride were dissolved in 300 ml of acetone, and a solution of 96.8 g of 1-naphthol in 300 ml of acetone was slowly added dropwise at 0° C. Subsequently, 168 ml of 4 N sodium hydroxide solution were slowly added dropwise. The mixture was stirred at 0° C. for 1 h, then warmed to room temperature and stirred for a further 1 h. The aqueous phase was removed and 200 ml of 5% NaOH and 200 ml of chloroform were added to the organic phase, the aqueous phase was removed again and the organic phase was washed twice with 80 ml each time of 5% NaOH and three times with 180 ml each time of water, and dried over sodium sulfate. The mixture was filtered and the solvent was distilled off under reduced pressure. The product was obtained as a colorless solid (preparation described in WO 8704321).

1. temperaturewarmed to room temperature
2. stirringstirred for a further 1 h
3. customThe aqueous phase was removed
4. addition200 ml of 5% NaOH and 200 ml of chloroform were added to the organic phase
5. customthe aqueous phase was removed again
6. washthe organic phase was washed twice with 80 ml each time of 5% NaOH and three times with 180 ml each time of water
7. dry with materialdried over sodium sulfate
8. filtrationThe mixture was filtered
9. distillationthe solvent was distilled off under reduced pressure
10. customThe product was obtained as a colorless solid (preparation described in WO 8704321)

ORD record

ord-dd67f260baeb4c4d845dabf2090ec54d

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09366957B2