Sulfuric Acid → Benzene, 1-(4-fluorophenoxy)-3-((2-(4-fluorophenyl)-2-methylbutoxy)methyl)-

HRID 1589446ノート

反応式

HRID 1589446 の反応式
C1(C)C=CC=CC=1.S(=O)(=O)(O)O.[F:13][C:14]1[CH:28]=[CH:27][C:17]([O:18][C:19]2[CH:20]=[C:21]([CH:24]=[CH:25][CH:26]=2)[CH2:22][OH:23])=[CH:16][CH:15]=1.[F:29][C:30]1[CH:35]=[CH:34][C:33]([C:36]([CH3:41])([CH2:39][CH3:40])[CH2:37]O)=[CH:32][CH:31]=1>O>[F:29][C:30]1[CH:35]=[CH:34][C:33]([C:36]([CH3:41])([CH2:39][CH3:40])[CH2:37][O:23][CH2:22][C:21]2[CH:24]=[CH:25][CH:26]=[C:19]([O:18][C:17]3[CH:27]=[CH:28][C:14]([F:13])=[CH:15][CH:16]=3)[CH:20]=2)=[CH:32][CH:31]=1

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 1140TolueneHCID 10584901[3-(4-Fluorophenoxy)phenyl]methanolHCID 155826502-(4-Fluorophenyl)-2-methylbutyl alcohol

生成物 1

HCID 3067111Benzene, 1-(4-fluorophenoxy)-3-((2-(4-fluorophenyl)-2-methylbutoxy)methyl)-収率 46%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To 20 ml of toluene were added 2 ml of concentrated sulfuric acid, 2.7 g of 3-(4-fluorophenoxy)benzyl alcohol and 2.3 g of 2-(4-fluorophenyl)-2-methylbutyl alcohol, and the mixture was refluxed for 6 hours (water formed by reaction was removed). The mixture was cooled to room temperature, and water was added to the mixture and the toluene layer was separated, washed with water, dried, and evaporated under reduced pressure, and the obtained crude ether was purified by column chromatography on 100 g of silica gel (1:1 mixed solvent of toluene and n-hexane was used as eluent) to give 2.2 g of the desired ether (the yield was 46% of the theoretical yield).

後処理

  1. temperaturethe mixture was refluxed for 6 hours
  2. customthe toluene layer was separated
  3. washwashed with water
  4. customdried
  5. customevaporated under reduced pressure
  6. customthe obtained crude ether
  7. customwas purified by column chromatography on 100 g of silica gel (1:1 mixed solvent of toluene and n-hexane was used as eluent)
  8. customto give 2.2 g of the desired ether (the yield was 46% of the
  9. customtheoretical yield)

出典と根拠

ORDレコード
ord-84a58df6590a49dbaeea8d5003bf041b
出典データセット
uspto-grants-1986_02
特許番号
US04570005

反応ノート

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