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Hydrochloric Acid → 3-(Methoxycarbonylmethyl)-4-isobutoxybenzoic acid

HRID 2249669
ノート
印刷プレビュー

反応式

HRID 2249669 の反応式
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([O:14][CH2:15][CH:16]([CH3:18])[CH3:17])=[C:7]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[CH:8]=1)=[O:2].P([O-])(O)(O)=[O:20].[Na+].OO.Cl([O-])=O.[Na+].Cl>C(#N)C.O.C(Cl)(Cl)Cl>[CH3:13][O:12][C:10]([CH2:9][C:7]1[CH:8]=[C:3]([CH:4]=[CH:5][C:6]=1[O:14][CH2:15][CH:16]([CH3:18])[CH3:17])[C:1]([OH:20])=[O:2])=[O:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 17816550Methyl 2-(5-formyl-2-isobutoxyphenyl)acetateHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

生成物 1

HCID 178165263-(Methoxycarbonylmethyl)-4-isobutoxybenzoic acid収率 72.8%

試薬・触媒・溶媒

3
HCID 962Water溶媒3 回HCID 6212Chloroform溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
7.5 °C

実験手順

In 8 ml of acetonitrile is dissolved 0.80 g of methyl 2-(5-formyl-2-isobutoxyphenyl)acetate. After successively adding 2.03 g of sodium dihydrogen-phosphate dissolved in 25 ml of water, 0.69 ml of 30% aqueous hydrogen peroxide and 0.73 g of sodium chlorite dissolved in 15 ml of water at a temperature of 5-10° C., the mixture thus obtained is stirred at 5-10° C. for 3.5 hours. Chloroform and water are added to the reaction mixture, pH is adjusted to 2.0 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 then the solvent is distilled off under reduced pressure. Thus, 0.62 g of 3-(methoxycarbonylmethyl)-4-isobutoxybenzoic acid is obtained as a colorless crystalline product.

後処理

  1. customthe mixture thus obtained
  2. customthe organic layer is separated
  3. customThe organic layer thus obtained
  4. washis washed with water and saturated aqueous solution of sodium chloride successively
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b6000604f322432fa50978a2d001169a
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

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