Potassium Carbonate → 4-Iodobenzophenone

HRID 496301

反応式

HRID 496301 の反応式
[IH:1].N[C:3]1[CH:16]=[CH:15][C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+]>CS(C)=O.CCOCC>[I:1][C:3]1[CH:16]=[CH:15][C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 143464-AminobenzophenoneHCID 24841Hydrogen iodide

生成物 1

HCID 5696384-Iodobenzophenone

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 3283Diethyl Ether溶媒

反応条件

温度
35 °C

実験手順

A solution of 57% aqueous HI (3.29 ml, 25 mmol) dissolved in DMSO (25 ml) was added dropwise to a solution of 4-aminobenzophenone (0.986 g, 5 mmol) in a mixture of 25 ml of DMSO and KNO2 (0.851 g, 10 mmol) at 35° C. with agitation. The added mixture was stirred at 35° C. for 10 minutes and then was transferred to a solution containing K2CO3 (5 g) in 100 ml ice-water. The reaction mixture was then taken up in ether, and then the ethereal extracts were washed with water and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure gave the crude 4-iodobenzophenone. The crude product was further purified by column chromatography to obtain 4-iodobenzophenone. The yield determined by gas chromatography was 88% (based on decane as an internal standard).

後処理

  1. washthe ethereal extracts were washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customRemoval of the solvent under reduced pressure
  4. customgave the crude 4-iodobenzophenone
  5. customThe crude product was further purified by column chromatography

出典と根拠

ORDレコード
ord-7a59f78b3b53467ba4027ed25d36eaab
出典データセット
uspto-grants-2005_09
特許番号
US06943257B2

関連ノート

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