Hydrochloric Acid → Methyl 2-[5-(4-isobutoxy-2-isopentyloxybenzoyl)-2-isobutoxyphenyl]acetate

HRID 2249626

反応式

HRID 2249626 の反応式
[OH:1][C:2]1[CH:25]=[C:24]([O:26][CH2:27][CH:28]([CH3:30])[CH3:29])[CH:23]=[CH:22][C:3]=1[C:4]([C:6]1[CH:7]=[CH:8][C:9]([O:17][CH2:18][CH:19]([CH3:21])[CH3:20])=[C:10]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:11]=1)=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH2:37](I)[CH2:38][CH:39]([CH3:41])[CH3:40].Cl>CN(C)C=O.O.C(OCC)(=O)C>[CH2:27]([O:26][C:24]1[CH:23]=[CH:22][C:3]([C:4]([C:6]2[CH:7]=[CH:8][C:9]([O:17][CH2:18][CH:19]([CH3:21])[CH3:20])=[C:10]([CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:11]=2)=[O:5])=[C:2]([O:1][CH2:37][CH2:38][CH:39]([CH3:41])[CH3:40])[CH:25]=1)[CH:28]([CH3:30])[CH3:29]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 109241-Iodo-3-methylbutaneHCID 11430Potassium CarbonateHCID 17816483HCID 17816483、化合物

生成物 1

HCID 17816460Methyl 2-[5-(4-isobutoxy-2-isopentyloxybenzoyl)-2-isobutoxyphenyl]acetate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

In 3 ml of N,N-dimethylformamide are suspended 0.28 g of methyl 2-[5-(2-hydroxy-4-isobutoxybenzoyl)-2-isobutoxyphenyl]acetate, 0.32 g of potassium carbonate and 0.23 ml of isopentyl iodide. The suspension is stirred at 120° C. for 2 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 6 mol/L hydrochloric acid, 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 0.17 g of methyl 2-[5-(4-isobutoxy-2-isopentyloxybenzoyl)-2-isobutoxyphenyl]-acetate as a colorless oily 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-ea1a440b465a47cda21db825488e9385
出典データセット
uspto-grants-2008_01
特許番号
US07314888B1

関連ノート

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