反応 #2503547

反応方程式

2,7-diacetyloxy-9-methylfluorene

lithium hydroxide monohydrate

hydrochloric acid

→

2,7-dihydroxy-9-methylfluorene

収率 84.2%

溶媒

ethylene glycol

反応条件

後処理

1. 1
   温度was refluxed for one hour
2. 2
   温度by heating
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The organic layer was sufficiently washed with water
5. 5
   乾燥dried on anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off from this organic layer under reduced pressure

実験手順

A mixture of 2,7-diacetyloxy-9-methylfluorene (12 g), lithium hydroxide monohydrate (3.42 g) and ethylene glycol (120 mL) was refluxed for one hour by heating. The reaction mixture was poured into 6M-hydrochloric acid and extracted with ethyl acetate. The organic layer was sufficiently washed with water and then dried on anhydrous magnesium sulfate. The solvent was distilled off from this organic layer under reduced pressure to obtain 2,7-dihydroxy-9-methylfluorene (7.24 g) of light brown crystal. Melting point: 191.5-196.3° C.

出典