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Methanol → 3-(3,4-Dimethoxyanilino)butanoic acid

HRID 597193
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반응식

HRID 597193 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[NH:6][CH:7]([CH3:14])[CH2:8][C:9]([O:11]CC)=[O:10].[OH-].[Na+].CO>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[NH:6][CH:7]([CH3:14])[CH2:8][C:9]([OH:11])=[O:10]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 21439734Ethyl 3-(3,4-dimethoxyanilino)butanoate

생성물 1

HCID 214397393-(3,4-Dimethoxyanilino)butanoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 54-g sample of the unpurified ester product of Example 2 was combined with 17.5 g of sodium hydroxide, 550 ml of methanol and 130 ml of water, and refluxed for 1.5 hrs. The reaction mixture was cooled, concentrated under reduced pressure, diluted with water and neutralized with 6N hydrochloric acid to give an oily mixture which was extracted with chloroform. The combined organic extracts were dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 48 g of an oily product. This material was used in the next step without further purification.

후처리

  1. temperaturerefluxed for 1.5 hrs
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure
  4. additiondiluted with water and neutralized with 6N hydrochloric acid
  5. customto give an oily mixture which
  6. extractionwas extracted with chloroform
  7. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-69595695bf724381ba0bd4fd93b2a8e6
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04013662

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