Sulfuric Acid → Methyl 9-hydroxy-9H-fluorene-9-carboxylate

HRID 33419

반응식

HRID 33419 반응식
[OH:1][C:2]1([C:15]([OH:17])=[O:16])[C:14]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.S(=O)(=O)(O)O.[C:23](=O)([O-])O.[Na+]>CO>[OH:1][C:2]1([C:15]([O:17][CH3:23])=[O:16])[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=2[C:9]2[C:14]1=[CH:13][CH:12]=[CH:11][CH:10]=2

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 10087FlurenolHCID 516892Sodium Bicarbonate

생성물 1

HCID 267210Methyl 9-hydroxy-9H-fluorene-9-carboxylate

시약·촉매·용매 1

HCID 887Methanol용매

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.

후처리

  1. temperaturerefluxed for 1 hour
  2. additionare added
  3. distillationthe methanol is largely distilled off under reduced pressure
  4. extractionThe residue remaining is extracted with dichloromethane and water
  5. customthe organic phase is dried
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0c0f7af10541490f902dc8554975b448
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429601B2

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