Potassium Carbonate → 3-(2-Chloro-4-trifluoromethoxyphenoxy)propanol

HRID 853924ノート

反応式

HRID 853924 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[CH:4][C:3]=1[OH:13].Br[CH2:15][CH2:16][CH2:17][OH:18].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:11])([F:12])[F:10])[CH:5]=[CH:4][C:3]=1[O:13][CH2:15][CH2:16][CH2:17][OH:18]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 130447832-Chloro-4-(trifluoromethoxy)phenol

生成物 1

HCID 685273763-(2-Chloro-4-trifluoromethoxyphenoxy)propanol収率 96%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 2-chloro-4-trifluoromethoxyphenol (16.4 g, 0.077 mole) in 100 mL of acetonitrile was added 3-bromopropanol (12.87 g, 0.092 mole) and potassium carbonate (21.33 g, 0.154 mole). The resulted solution was refluxed at 75° C.-80° C. overnight. The solvent was then evaporated. The residue was dissolved in 100 mL of ethyl acetate and washed with 100 mL of H2O. The organic layer was separated, dried over MgSO4, filtered and the organic solvent was evaporated to yield 20 g of the product.

後処理

  1. temperatureThe resulted solution was refluxed at 75° C.-80° C. overnight
  2. customThe solvent was then evaporated
  3. dissolutionThe residue was dissolved in 100 mL of ethyl acetate
  4. washwashed with 100 mL of H2O
  5. customThe organic layer was separated
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customthe organic solvent was evaporated

出典と根拠

ORDレコード
ord-b8f2ef0292654eec9fe9e91d70926c9b
出典データセット
uspto-grants-2007_08
特許番号
US07256218B2

反応ノート

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