반응 #10463

반응 방정식

9-hydroxy-9-fluorenecarboxylic acid

sulphuric acid

sodium hydrogen carbonate

→

methyl 9-hydroxy-fluorene-9-carboxylate

용매

methanol

반응 조건

후처리

1. 1
   온도refluxed for 1 hour
2. 2
   workup.ADDITIONare added
3. 3
   workup.DISTILLATIONthe methanol is largely distilled off under reduced pressure
4. 4
   추출The residue remaining is extracted with dichloromethane and water
5. 5
   기타the organic phase is dried
6. 6
   기타evaporated to dryness

실험 절차

50.4 g (0.223 mol) 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 ml of methanol, combined with 5 ml (0.089 mol) conc. sulphuric acid and refluxed for 1 hour. After cooling 100 ml sodium hydrogen carbonate solution (about pH 8) are added, and the methanol is largely distilled off under reduced pressure. The residue remaining is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness.

출처