Ethylene carbonate → 4-(2-Hydroxyethoxyphenyl)fluorene

HRID 789

반응식

HRID 789 반응식
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

참가 물질

5

반응물 4

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

생성물 1

HCID 232084214-(2-Hydroxyethoxyphenyl)fluorene수율 970.1%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bfcf42b524d14d69860f018538be3094
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723264

연결된 노트

불러오는 중…