Potassium Iodide → Methyl (m-[m-phenoxyphenoxy]phenoxy)-alpha-[p-(p-chlorophenoxy)phenyl]acetate

HRID 1863300ノート

反応式

HRID 1863300 の反応式
[O:1]([C:8]1[CH:9]=[C:10]([CH:19]=[CH:20][CH:21]=1)[O:11][C:12]1[CH:13]=[C:14]([OH:18])[CH:15]=[CH:16][CH:17]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O-].[Na+].[I-].[K+].Br[CH:28]([C:33]1[CH:38]=[CH:37][C:36]([O:39][C:40]2[CH:45]=[CH:44][C:43]([Cl:46])=[CH:42][CH:41]=2)=[CH:35][CH:34]=1)[C:29]([O:31][CH3:32])=[O:30]>CO.C1C=CC=CC=1.O>[O:1]([C:8]1[CH:9]=[C:10]([CH:19]=[CH:20][CH:21]=1)[O:11][C:12]1[CH:13]=[C:14]([CH:15]=[CH:16][CH:17]=1)[O:18][CH:28]([C:33]1[CH:38]=[CH:37][C:36]([O:39][C:40]2[CH:41]=[CH:42][C:43]([Cl:46])=[CH:44][CH:45]=2)=[CH:35][CH:34]=1)[C:29]([O:31][CH3:32])=[O:30])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

8

反応物 4

HCID 4875Potassium IodideHCID 84251Phenol, 3-(3-phenoxyphenoxy)-HCID 10942334Sodium MethoxideHCID 20392594Methyl alpha-Bromo-alpha-[p-(p-chlorophenoxy)phenyl]acetate

生成物 1

HCID 86736645Methyl (m-[m-phenoxyphenoxy]phenoxy)-alpha-[p-(p-chlorophenoxy)phenyl]acetate

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 6.96 g of m-(m-phenoxyphenoxy)phenol, 1.19 g of sodium methoxide and 50 mg of potassium iodide in 40 ml of methanol is added 7.11 g of methyl α-bromo-α-[p-(p-chlorophenoxy)phenyl]acetate in 10 ml of benzene. The mixture is refluxed for 20 hours, poured into ice and water and extracted with chloroform. The chloroform extracts are washed with 10% potassium carbonate and with water. The extract is dried over magnesium sulfate and concentrated under vacuum to give an oil. Filtration once through silica gel (chloroform solvent) and again through silica gel with benzene as solvent gives the product as an oil.

後処理

  1. temperatureThe mixture is refluxed for 20 hours
  2. extractionextracted with chloroform
  3. washThe chloroform extracts are washed with 10% potassium carbonate and with water
  4. dry with materialThe extract is dried over magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. customto give an oil
  7. filtrationFiltration once through silica gel (chloroform solvent)

出典と根拠

ORDレコード
ord-bda675eb7dbd4415a813c129aea4875b
出典データセット
uspto-grants-1979_09
特許番号
US04168385

反応ノート

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