Potassium Carbonate → 4-fluoronaphthalen-1-ol

HRID 2062055노트

반응식

HRID 2062055 반응식
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

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 23132789HCID 23132789, 화합물

생성물 1

HCID 109208304-fluoronaphthalen-1-ol수율 92%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-823162d8a0dd49fd926d8bde916ab4c2
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283479B2

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