Sodium Chloride → 2-Fluorotetracene-5,12-dione

HRID 745895

반응식

HRID 745895 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[Cl-].[Na+].[F:7][C:8]1[CH:28]=[CH:27][C:11]([C:12]([C:14]2[C:23]([C:24]([OH:26])=O)=[CH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=2)=[O:13])=[CH:10][CH:9]=1>>[F:7][C:8]1[CH:28]=[CH:27][C:11]2[C:12](=[O:13])[C:14]3[C:23](=[CH:22][C:21]4[C:16]([CH:15]=3)=[CH:17][CH:18]=[CH:19][CH:20]=4)[C:24](=[O:26])[C:10]=2[CH:9]=1

참가 물질

4

반응물 3

HCID 5234Sodium ChlorideHCID 6451240Aluminum(III) ChlorideHCID 233109402-(4-Fluorobenzoyl)-naphthalene-3-carboxylic acid

생성물 1

HCID 200898282-Fluorotetracene-5,12-dione수율 70%

실험 절차

200 g (1.5 moles) of powdered aluminium chloride and 40 g (684 mmol) of sodium chloride are heated together at 140°-150° C. After about 1.5 hours, 40 g (136 mmol) of 2-(4-fluorobenzoyl)-naphthalene-3-carboxylic acid are added to the melt. The dark red mixture is stirred at 140°-150° C. for one hour. Hydrolysis is then carried out at about 100° C. by slowly adding ice-water. The precipitate is filtered off and stirred with 10% sodium carbonate solution. It is then washed neutral with water and dried. The resulting product is sublimed at 230° C. 13.1 g (70% of theory) of 2-fluoro-5,12-naphthacenequinone are obtained.

후처리

  1. customHydrolysis
  2. filtrationThe precipitate is filtered off
  3. stirringstirred with 10% sodium carbonate solution
  4. washIt is then washed neutral with water
  5. customdried
  6. customis sublimed at 230° C

출처 및 근거

ORD 기록
ord-097af5c0522e4de0b85d444c5265758a
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04601853

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