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

HRID 2249669
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HRID 2249669 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

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

생성물 1

HCID 178165263-(Methoxycarbonylmethyl)-4-isobutoxybenzoic acid수율 72.8%

시약·촉매·용매

3
HCID 962Water용매3회HCID 6212Chloroform용매HCID 6342Acetonitrile용매

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온도
7.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b6000604f322432fa50978a2d001169a
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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