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

HRID 33419

反応式

HRID 33419 の反応式
[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

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 10087FlurenolHCID 516892Sodium Bicarbonate

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0c0f7af10541490f902dc8554975b448
出典データセット
uspto-grants-2008_09
特許番号
US07429601B2

関連ノート

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