Ethylene carbonate → 4-(2-Hydroxyethoxyphenyl)fluorene

HRID 789

反応式

HRID 789 の反応式
OC1[CH:7]=[CH:6][C:5]([C:8]2([C:21]3[CH:26]=CC(O)=CC=3)[C:20]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[C:14]3C2=[CH:10][CH:11]=[CH:12][CH:13]=3)=[CH:4]C=1.C1(=O)O[CH2:31][CH2:30][O:29]1.[C:34](=[O:37])([O-])[O-].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>>[OH:29][CH2:30][CH2:31][O:37][C:34]1[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=1[C:15]1[C:20]2[C:8]3[C:5](=[CH:6][CH:7]=[CH:26][CH:21]=3)[CH2:4][C:19]=2[CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 4

HCID 7303Ethylene carbonateHCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 767169,9-Bis(4-hydroxyphenyl)fluorene

生成物 1

HCID 232084214-(2-Hydroxyethoxyphenyl)fluorene収率 970.1%

実験手順

A mixture of 84.4 g (0.241 mol) of 9,9-bis(4-hydroxyphenyl)fluorene, 46.7 g (0.53 mol) of ethylene carbonate, 3.3 g (0.024 mol) of potassium carbonate, and a catalytic amount of 18-crown-6 in 400 mL of xylenes was heated at reflux with mechanical stirring for 6 h. The mixture was allowed to cool slowly to room temperature, and the solvent was decanted from the precipitated product. The resulting white solid was washed with ligroin (to prevent the formation of a gummy mass), and dried under a stream of nitrogen. The product was recrystallized from methanol, providing 70.4 g (67%) of a white powder.

後処理

  1. temperatureat reflux
  2. customthe solvent was decanted from the precipitated product
  3. washThe resulting white solid was washed with ligroin (
  4. customdried under a stream of nitrogen
  5. customThe product was recrystallized from methanol

出典と根拠

ORDレコード
ord-bfcf42b524d14d69860f018538be3094
出典データセット
uspto-grants-1998_03
特許番号
US05723264

関連ノート

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