Chloroform → Methyl 2-[5-(2-hydroxy-4-isobutoxybenzoyl)-2-isobutoxyphenyl]acetate

HRID 2249625ノート

反応式

HRID 2249625 の反応式
C([O:5][C:6]1[CH:29]=[C:28]([O:30][CH2:31][CH:32]([CH3:34])[CH3:33])[CH:27]=[CH:26][C:7]=1[C:8]([C:10]1[CH:11]=[CH:12][C:13]([O:21][CH2:22][CH:23]([CH3:25])[CH3:24])=[C:14]([CH2:16][C:17]([O:19][CH3:20])=[O:18])[CH:15]=1)=[O:9])C(C)C.[Cl-].[Al+3].[Cl-].[Cl-].C(Cl)(Cl)Cl>C(Cl)Cl>[OH:5][C:6]1[CH:29]=[C:28]([O:30][CH2:31][CH:32]([CH3:34])[CH3:33])[CH:27]=[CH:26][C:7]=1[C:8]([C:10]1[CH:11]=[CH:12][C:13]([O:21][CH2:22][CH:23]([CH3:25])[CH3:24])=[C:14]([CH2:16][C:17]([O:19][CH3:20])=[O:18])[CH:15]=1)=[O:9]

参加物

5

反応物 3

HCID 6212ChloroformHCID 6451240Aluminum(III) ChlorideHCID 17816545Methyl 2-[5-(2,4-diisobutoxybenzoyl)-2-isobutoxyphenyl]acetate

生成物 1

HCID 17816483Methyl 2-[5-(2-hydroxy-4-isobutoxybenzoyl)-2-isobutoxyphenyl]acetate収率 46.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 15 ml of methylene chloride is dissolved 1.50 g of methyl 2-[5-(2,4-diisobutoxybenzoyl)-2-isobutoxyphenyl]acetate, to which is added 1.06 g of aluminum chloride at ambient temperature. The mixture is stirred at ambient temperature for 2 hours. The reaction mixture is added to a mixture of chloroform and ice water, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1) to obtain 0.62 g of methyl 2-[5-(2-hydroxy-4-isobutoxybenzoyl)-2-isobutoxyphenyl]acetate as a yellow-colored solid product.

後処理

  1. customthe organic layer is separated
  2. customThe organic layer thus obtained
  3. washis washed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure
  6. customThe residue thus obtained
  7. customis purified by silica gel column chromatography (eluent; hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-02338cb65c1e400eafd637a95a8bb9bf
出典データセット
uspto-grants-2008_01
特許番号
US07314888B1

反応ノート

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