Hydrochloric Acid → 11-(3,5-Bis(trifluoromethyl) phenoxy)dodecanoic acid

HRID 1363868ノート

反応式

HRID 1363868 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([OH:13])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.Br[CH:17]([CH3:30])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([OH:29])=[O:28].Cl>[OH-].[Na+]>[F:1][C:2]([F:14])([F:15])[C:3]1[CH:4]=[C:5]([CH:6]=[C:7]([C:9]([F:11])([F:10])[F:12])[CH:8]=1)[O:13][CH:17]([CH3:30])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([OH:29])=[O:28]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 676803,5-Bis(trifluoromethyl)phenolHCID 531294511-Bromododecanoic acid

生成物 1

HCID 8662056111-(3,5-Bis(trifluoromethyl) phenoxy)dodecanoic acid収率 255.2%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

3,5-Bis(trifluoromethyl) phenol (20.6 g) was dissolved in 1N sodium hydroxide (270 mL). The solution was refluxed under heating for 10 hours. Further, the solution was added with 11-bromododecanoic acid (4.7 g). After the reflux under heating was continued, the reaction solution was left to be cooled. The reaction solution was added with 1N aqueous hydrochloric acid and extracted with ethyl acetate. The resulting organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed. The resulting crystals was washed with hexane and purified by silica gel column chromatography to obtain 11-(3,5-Bis(trifluoromethyl) phenoxy)dodecanoic acid (18.4 g, 50%).

後処理

  1. temperatureThe solution was refluxed
  2. temperatureunder heating for 10 hours
  3. temperatureAfter the reflux
  4. temperatureunder heating
  5. waitthe reaction solution was left
  6. temperatureto be cooled
  7. extractionextracted with ethyl acetate
  8. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. washThe resulting crystals was washed with hexane
  11. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-8166c470559342e5b823bd2e576321b5
出典データセット
uspto-grants-2011_02
特許番号
US07887835B2

反応ノート

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