Réaction #660210

Équation de réaction

docosyl bromide

potassium carbonate

docosyl bromide

2,7-Dihydroxy-9-fluorenone

hydrochloric acid

→

2,7-didocosyloxy-9-fluorenone

Rendement 107.5%

Solvants

DMF

Conditions de réaction

Traitement

1. 1
   workup.STIRRINGthe mixture was stirred overnight
2. 2
   AutreAfter completion of the reaction
3. 3
   Températurethe reaction mixture was cooled to room temperature
4. 4
   Autrein a water bath to allow
5. 5
   Autreprecipitation
6. 6
   FiltrationThe crystals were collected by filtration and slurry
7. 7
   Lavagewashed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml)

Mode opératoire

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).

Source