Potassium Carbonate → 4-fluoronaphthalen-1-ol

HRID 2075487ノート

反応式

HRID 2075487 の反応式
C([O:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([F:15])=[CH:7][CH:6]=1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O>[F:15][C:8]1[C:9]2[C:14](=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5]([OH:4])=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 23132789HCID 23132789、化合物

生成物 1

HCID 109208304-fluoronaphthalen-1-ol収率 92%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a stirred solution of 2.71 g of 1-acetoxy-4-fluoro-naphthalene in 142 ml of degassed methanol was added a solution of 9.2 g of potassium carbonate in 95 ml of degassed water. The mixture was stirred at room temperature for 5 h. The mixture was cooled with ice, acidified to pH1-2 with conc. HCL, extracted with dichloromethane, dried (magnesium sulphate), filtered and concentrated to an orange solid. The material was purified by chromatography on silica gel eluting with dichloromethane/heptanes/toluene to provide 1.98 g of 4-fluoro-1-hydroxynaphthalene as a white solid.

後処理

  1. temperatureThe mixture was cooled with ice
  2. extractionextracted with dichloromethane
  3. dry with materialdried (magnesium sulphate)
  4. filtrationfiltered
  5. concentrationconcentrated to an orange solid
  6. customThe material was purified by chromatography on silica gel eluting with dichloromethane/heptanes/toluene

出典と根拠

ORDレコード
ord-a1dfb7593ab9405082e3c5ccaf4fcac1
出典データセット
uspto-grants-2011_04
特許番号
US07919628B2

反応ノート

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