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

HRID 597193
ノート
印刷プレビュー

反応式

HRID 597193 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-69595695bf724381ba0bd4fd93b2a8e6
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04013662

反応ノート

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