2-Bromoethanol → 2-(4-Bromo-2-(trifluoromethyl)phenoxy)-ethanol

HRID 518000ノート

反応式

HRID 518000 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:20][CH2:21][OH:22]>C(#N)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:20][CH2:21][OH:22])=[C:4]([C:9]([F:10])([F:11])[F:12])[CH:3]=1

参加物

5

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 142784o-Cresol, 4-bromo-alpha,alpha,alpha-trifluoro-

生成物 1

HCID 576575832-(4-Bromo-2-(trifluoromethyl)phenoxy)-ethanol

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4-Bromo-2-(trifluoromethyl)phenol (83 mmol, 20 g), potassium carbonate (166 mmol, 22.94 g) and 2-bromoethanol (124 mmol, 8.79 mL, 15.56 g) were combined and heated to reflux for overnight in Acetonitrile (200 mL). The reaction mixture was washed with water, 0.5M NaOH, dried over sodium sulfate and concentrated in vacuo. The resulting residue was taken up in hot heptane (300 mL) and allowed to crystallise. The solid was filtered off to afford 2-(4-bromo-2-(trifluoromethyl)-phenoxy)ethanol. (20.74 g)

後処理

  1. temperatureheated
  2. washThe reaction mixture was washed with water, 0.5M NaOH
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto crystallise
  6. filtrationThe solid was filtered off

出典と根拠

ORDレコード
ord-5de1fadde5dc471da8087ce9ea939a0e
出典データセット
uspto-grants-2015_08
特許番号
US09115126B2

反応ノート

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