4-Fluorophenol → 6-Fluoro-2-methyl-4-chromanone

HRID 868535노트

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HRID 868535 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[C:9](O)(=[O:13])/[CH:10]=[CH:11]/[CH3:12].[OH-].[Na+]>>[F:1][C:2]1[CH:7]=[C:6]2[C:5](=[CH:4][CH:3]=1)[O:8][CH:11]([CH3:12])[CH2:10][C:9]2=[O:13]

참가 물질

4

반응물 3

HCID 97324-FluorophenolHCID 14798Sodium HydroxideHCID 637090Crotonic Acid

생성물 1

HCID 27373906-Fluoro-2-methyl-4-chromanone

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온도
120 °C

실험 절차

11.2 G (0.1 mol) of para-fluorophenol and 17.2 g (0.2 mol) of crotonic acid were dissolved in 100 ml of polyphosphoric acid, and the solution was reacted with vigorously stirring at 120° C. for 8 hours. After cooling, the reaction solution was poured into 450 ml of iced 2N-sodium hydroxide solution, and the mixture was extracted with 500 ml of chloroform. The chloroform layer was washed with 2N-sodium hydroxide solution and with water, followed by drying over magnesium sulfate. The solvent was distilled off, and the residue was recrystallized from n-hexane in the amount of about ten times. There were thus obtained 5.8 g (yield : 32%) of the subject material, 6-fluoro-2-methyl-4- chromanone.

후처리

  1. customthe solution was reacted
  2. temperatureAfter cooling
  3. extractionthe mixture was extracted with 500 ml of chloroform
  4. washThe chloroform layer was washed with 2N-sodium hydroxide solution and with water
  5. dry with materialby drying over magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was recrystallized from n-hexane in the amount of about ten times

출처 및 근거

ORD 기록
ord-65487d07f7f24ca59ba0760bf2d3df6d
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04780472

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