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Potassium Iodide → HCID 23371333、化合物

HRID 1735703
ノート
印刷プレビュー

反応式

HRID 1735703 の反応式
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[S:6][CH:7]=1.[OH:15][CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:18].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(O)C>[F:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]2[S:6][CH:7]=[C:3]([CH2:2][O:15][CH2:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:18])[N:4]=2)=[CH:9][CH:10]=1
参加物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 4875Potassium IodideHCID 11430Potassium CarbonateHCID 68490alpha-HydroxyacetophenoneHCID 21108384-(chloromethyl)-2-(4-fluorophenyl)-1,3-thiazole

生成物 1

HCID 23371333HCID 23371333、化合物収率 74.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

11.2 g (0.05 mol) of 4-chloromethyl-2-(4-fluorophenyl) thiazole (see Example 4), 5.4 g (0.04 mol) of 2-hydroxyacetophenone, 7.5 g (0.055 mol) of potassium carbonate and 0.5 g of potassium iodide in 20 ml ethanol are refluxed for 24 hours. The mixture is filtered, the filtrate is concentrated, the residue is taken up in dichloromethane, the solution is extracted with dilute sodium hydroxide solution and then with water, and the organic phase is dried over MgSO4. Removal of the solvent by distillation under reduced pressure results in a solid residue which is washed with diisopropyl ether to give 9.7 g (59% yield) of 2-[2-(4-fluorophenyl)-4-thiazolylmethyloxy]acetophenone as yellowish crystals of melting point 104°-106° C.

後処理

  1. filtrationThe mixture is filtered
  2. concentrationthe filtrate is concentrated
  3. extractionthe solution is extracted with dilute sodium hydroxide solution
  4. dry with materialwith water, and the organic phase is dried over MgSO4
  5. customRemoval of the solvent
  6. distillationby distillation under reduced pressure
  7. customresults in a solid residue which
  8. washis washed with diisopropyl ether

出典と根拠

ORDレコード
ord-6b7ee6a66c2a47a49a99a96d1d3bf3f4
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05538940

反応ノート

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