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Aluminum(III) Chloride → HCID 10360821, 화합물

HRID 1607673
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HRID 1607673 반응식
[F:1][C:2]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[C:8](Cl)=[O:9].[Cl-].[Al+3].[Cl-].[Cl-]>C1C=CC=CC=1>[F:1][C:2]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[C:8]([C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:3]=1)=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 10448313HCID 10448313, 화합물

생성물 1

HCID 10360821HCID 10360821, 화합물수율 184.6%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

A mixture of 3-(2,4-difluorophenoxy)-4-nitrobenzoic acid (2.1 g) and phosphorus pentachloride (1.6 g) in benzene (20 ml) was stirred for 2 hours at room temperature. The mixture was concentrated under reduced pressure to give crystals of 3-(2,4-difluorophenoxy)-4-nitrobenzoyl chloride (2.2 g). A solution of 3-(2,4-difluorophenoxy)-4-nitrobenzoyl chloride (2.2 g) in benzene (20 ml) was added to a mixture of aluminum chloride (2.4 g) in benzene (20 ml). The mixture was stirred overnight at ambient temperature and concentrated under reduced pressure. The residue was dissolved in chloroform, washed with diluted hydrochloric acid and water successively, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from a mixture of hexane and ethanol to give crystals of 3-(2,4-difluorophenoxy)-4-nitrobenzophenone (2.3 g).

후처리

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in chloroform
  3. washwashed with diluted hydrochloric acid and water successively
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from a mixture of hexane and ethanol

출처 및 근거

ORD 기록
ord-1cff1bf665124f5d8db33a18575e39aa
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04866091

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