Hydrochloric Acid → 2,7-Didocosyloxy-9-fluorenone

Temperatur

80 °C

2,7-Dihydroxy-9-fluorenone (1 g, 4.71 mmol) was dissolved in DMF (40 ml), and potassium carbonate (1.95 g, 14.1 mmol) and docosyl bromide (96%, 4.02 g, 9.91 mmol) were added. The mixture was stirred overnight at 80° C., docosyl bromide (0.40 g, 0.99 mmol) was further added and the mixture was stirred overnight. After completion of the reaction, the reaction mixture was cooled to room temperature, 1N hydrochloric acid (120 ml) was added thereto in a water bath to allow precipitation. The crystals were collected by filtration and slurry washed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml) to give 2,7-didocosyloxy-9-fluorenone (4.20 g, docosyl bromide mixture).

1. stirringthe mixture was stirred overnight
2. customAfter completion of the reaction
3. temperaturethe reaction mixture was cooled to room temperature
4. customin a water bath to allow
5. customprecipitation
6. filtrationThe crystals were collected by filtration and slurry
7. washwashed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml)

ORD-Eintrag

ord-4b2220a64d72410ba99bbe69369cf75f

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09029504B2