反応 #660210

反応方程式

docosyl bromide

potassium carbonate

docosyl bromide

2,7-Dihydroxy-9-fluorenone

hydrochloric acid

→

2,7-didocosyloxy-9-fluorenone

収率 107.5%

溶媒

DMF

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred overnight
2. 2
   その他After completion of the reaction
3. 3
   温度the reaction mixture was cooled to room temperature
4. 4
   その他in a water bath to allow
5. 5
   その他precipitation
6. 6
   ろ過The crystals were collected by filtration and slurry
7. 7
   洗浄washed once with 1N hydrochloric acid (40 ml), once with pure water (40 ml) and once with methanol (40 ml)

実験手順

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).

出典