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

HRID 1589446노트

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HRID 1589446 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-84a58df6590a49dbaeea8d5003bf041b
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04570005

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