ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzoyl chloride → Methanone, (2-chlorophenyl)phenyl-

HRID 890852
ノート
印刷プレビュー

反応式

HRID 890852 の反応式
[N-](S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O.[N-](S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O.C([N+]1C=CN(C)C=1)CCC.C([N+]1C=CN(C)C=1)CCC.[Cl:51][C:52]1[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=1.[C:58](Cl)(=[O:65])[C:59]1[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=1>N(S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O.N(S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O.[Ni+2]>[Cl:51][C:52]1[CH:57]=[CH:56][CH:55]=[CH:54][C:53]=1[C:58]([C:59]1[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=1)=[O:65]
参加物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 7412Benzoyl chlorideHCID 7964ChlorobenzeneHCID 178448536HCID 178448536、化合物

生成物 1

HCID 78838Methanone, (2-chlorophenyl)phenyl-収率 76.2%

試薬・触媒・溶媒 1

HCID 131725278Nickel(II) bis-triflimide触媒

実験手順

Nickel(II) bis-triflimide (0.062 g, 0.1 mmol) was added to 1-butyl-3-methylimidazolium bis-trifluoromethanesulfonimide ([bmim][NTf2]) (1.0 g) in a 25 cm3 round-bottomed flask equipped with a magnetic stirrer and reflux condenser, and the mixture stirred until the catalyst dissolved. Chlorobenzene (1.68 g, 15 mmol) and benzoyl chloride (1.41 g, 10 mmol) were added. The mixture was heated under reflux for 72 hours and was analysed by gas chromatographic analysis as in previous examples. The reaction was cooled to room temperature. Petroleum ether (15 cm3, bp=40-60° C.) was added and the catalyst and ionic liquid formed a separate phase from the petroleum ether layer. The solution of the product (in petroleum ether) was decanted and the flask (containing the ionic liquid and catalyst) washed three times with 15 cm3 of petroleum ether. Concentration of the organic extract, followed by Kugenrohr distillation at 1 mm Hg (bp=170-190° C.), gave chlorobenzophenone (1.65 g, 74%). GC analysis showed 78% yield after 72 hours, with a 70:8 4- to 2- isomer ratio. This is a remarkable result, as chlorobenzene is known to be classically unreactive in acylation reactions. It has not previously been possible to isolate significant quantities of the products of the acylation of chlorobenzene.

後処理

  1. customequipped with a magnetic stirrer
  2. temperaturereflux condenser
  3. dissolutiondissolved
  4. temperatureThe mixture was heated
  5. temperatureunder reflux for 72 hours
  6. customThe solution of the product (in petroleum ether) was decanted
  7. additionthe flask (containing the ionic liquid and catalyst)
  8. washwashed three times with 15 cm3 of petroleum ether
  9. distillationConcentration of the organic extract, followed by Kugenrohr distillation at 1 mm Hg (bp=170-190° C.)

出典と根拠

ORDレコード
ord-552be1ab3b374393abac31bd334ea2a1
出典データセット
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06998497B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート