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Sulfuric Acid → 5-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one

HRID 1648185
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인쇄 미리보기

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HRID 1648185 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]([C:12]([CH3:14])=[O:13])[C:9]([OH:11])=[O:10].C(O[C:19](=O)[CH3:20])(=O)C.S(=O)(=O)(O)O.[C:27](=O)([O-])[O-].[Na+].[Na+]>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9](=[O:11])[O:10][C:19]([CH3:20])([CH3:27])[O:13][C:12]=1[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 3023024Acetyl(2-fluorophenyl)acetic acid

생성물 1

HCID 153008465-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2-(2-fluorophenyl)acetoacetic acid (5.1 g), acetone (4.2 ml), and acetic anhydride (5.4 ml) was kept at -20° C. and concentrated sulfuric acid (0.3 ml) was added thereto. This was kept at -15° C. and the reaction was carried out for 48 hours. The reaction mixture was added to an aqueous 10 % sodium carbonate solution (150 ml) which was ice-cooled, and the mixture was stirred for a short time at room temperature. White crystals which formed were collected by filtration, and washed well with water and then with hexane. The crystals obtained were dried well under reduced pressure to obtain the captioned compound (5.2 g).

후처리

  1. customwas kept at -20° C.
  2. customThis was kept at -15° C.
  3. temperaturecooled
  4. customWhite crystals which formed
  5. filtrationwere collected by filtration
  6. washwashed well with water
  7. customThe crystals obtained
  8. customwere dried well under reduced pressure

출처 및 근거

ORD 기록
ord-bdc3e776827c407685d5ec95f971d9c4
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05436224

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