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Hydrochloric Acid → (4-Fluoro-3-nitrophenyl)(phenyl)methanone

HRID 2248320
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인쇄 미리보기

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HRID 2248320 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[F:5][C:6]1[CH:14]=[CH:13][C:9]([C:10](Cl)=[O:11])=[CH:8][C:7]=1[N+:15]([O-:17])=[O:16].Cl>C1C=CC=CC=1>[F:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([C:6]2[CH:14]=[CH:13][CH:9]=[CH:8][CH:7]=2)=[O:11])=[CH:8][C:7]=1[N+:15]([O-:17])=[O:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 27833474-Fluoro-3-nitrobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 14590583(4-Fluoro-3-nitrophenyl)(phenyl)methanone수율 73%

시약·촉매·용매 1

HCID 241Benzene용매2회

반응 조건

온도
60 °C

실험 절차

To a stirred mixture of 496 parts of aluminum chloride in 900 parts of benzene was added dropwise a solution of 256 parts of 4-fluoro-3-nitrobenzoyl chloride in 225 parts of benzene at ±10° C. Upon complete addition, stirring was continued first for 1.5 hours in an ice bath and then for 8 hours at room temperature. The mixture was heated to 60° C., cooled again and poured into crushed ice and 180 parts of concentrated hydrochloric acid. The separated organic layer was dried, filtered and concentrated. The concentrate was dissolved in 2100 parts of 2,2'-oxybispropane, the solution was treated with diatomaceous earth and activated charcoal. After filtration, the filtrate was concentrated. The crystallized product was filtered off and dried, yielding 223 parts (73%) of (4-fluoro-3-nitrophenyl) phenylmethanone; mp. 59° C. (int. 62).

후처리

  1. additionUpon complete addition
  2. waitfor 8 hours at room temperature
  3. temperaturecooled again
  4. additionpoured
  5. customThe separated organic layer was dried
  6. filtrationfiltered
  7. concentrationconcentrated
  8. dissolutionThe concentrate was dissolved in 2100 parts of 2,2'-oxybispropane
  9. additionthe solution was treated with diatomaceous earth and activated charcoal
  10. filtrationAfter filtration
  11. concentrationthe filtrate was concentrated
  12. filtrationThe crystallized product was filtered off
  13. customdried

출처 및 근거

ORD 기록
ord-37971e1e561f45958702221b1709b7b4
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05039677

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