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

HRID 2248320
ノート
印刷プレビュー

反応式

HRID 2248320 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-37971e1e561f45958702221b1709b7b4
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05039677

反応ノート

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