Potassium Carbonate → 1-(5'-Ethoxymethoxy-2'methyl-2-propylbiphenyl-4-yl)propan-1-one

HRID 584287ノート

反応式

HRID 584287 の反応式
[CH2:1]([O:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:15])=[C:10](B(O)O)[CH:11]=1)[CH3:2].FC(F)(F)S(O[C:22]1[CH:27]=[CH:26][C:25]([C:28](=[O:31])[CH2:29][CH3:30])=[CH:24][C:23]=1[CH2:32][CH2:33][CH3:34])(=O)=O.[Cl-].[Li+].C(=O)([O-])[O-].[K+].[K+]>COCCOC.O>[CH2:1]([O:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:15])=[C:10]([C:22]2[CH:27]=[CH:26][C:25]([C:28](=[O:31])[CH2:29][CH3:30])=[CH:24][C:23]=2[CH2:32][CH2:33][CH3:34])[CH:11]=1)[CH3:2]

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 433294Lithium ChlorideHCID 223456045-Ethoxymethoxy-2-methylphenylboronic acidHCID 223456254-Propionyl-2-propylphenyl 1,1,1-trifluoromethanesulfonate

生成物 1

HCID 223456341-(5'-Ethoxymethoxy-2'methyl-2-propylbiphenyl-4-yl)propan-1-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

1.56 g (7.4 mmol) of 5-ethoxymethoxy-2-methylphenylboronic acid, 2 g (6.2 mmol) of 4-propionyl-2-propylphenyl 1,1,1-trifluoromethanesulfonate, 517 mg (12 mmol) of lithium chloride and 7.4 ml of 2M potassium carbonate solution are dissolved in 50 ml of 1,2-dimethoxyethane in a round-bottomed flask and under a stream of nitrogen. The mixture is refluxed for 10 hours. It is then poured into water and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered and then evaporated. A brown oil is obtained, which is used without further purification for the rest of the synthesis.

後処理

  1. temperatureThe mixture is refluxed for 10 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customA brown oil is obtained
  7. customwhich is used without further purification for the rest of the synthesis

出典と根拠

ORDレコード
ord-38af767a9938472f8beb49ae44c4f95f
出典データセット
uspto-grants-2005_08
特許番号
US06924400B2

反応ノート

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