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Potassium Carbonate → t-Butyl (3-iodophenoxy)acetate

HRID 1352867
ノート
印刷プレビュー

反応式

HRID 1352867 の反応式
[I:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18].S([O-])(O)(=O)=O.[K+]>CN(C)C=O>[I:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18]
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

6

反応物 4

HCID 11430Potassium CarbonateHCID 122723-IodophenolHCID 79177tert-Butyl bromoacetateHCID 516920Potassium bisulfate

生成物 1

HCID 52449400t-Butyl (3-iodophenoxy)acetate収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a solution of m-iodophenol (1.22 g, 5.55 mmol) in N,N-dimethylformamide (15 ml) were added potassium carbonate (1.40 g, 10.1 mmol) and t-butyl bromoacetate (1.22 ml, 6.25 mmol), and the mixture was stirred for 3 hours at 50° C. Thereto was added an aqueous 5% potassium hydrogensulfate solution and the mixture was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated sodium chloride solution, and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue was purified with silica gel chromatography (hexane:ethyl acetate=4:1) to give the subject compound (1.85 g, 100%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with an aqueous saturated sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified with silica gel chromatography (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-e1b41d7ca33e47caad642e24bc40dcae
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220773B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート