3,4-Dichloroaniline → 3-(3,4-Dichloroanilino)butanoic acid

HRID 2413957

反応式

HRID 2413957 の反応式
[C:1]1(=[O:6])[O:5][CH:3]([CH3:4])[CH2:2]1.[Cl:7][C:8]1[CH:9]=[C:10]([CH:12]=[CH:13][C:14]=1[Cl:15])[NH2:11]>CCOCC>[Cl:7][C:8]1[CH:9]=[C:10]([CH:12]=[CH:13][C:14]=1[Cl:15])[NH:11][CH:3]([CH3:4])[CH2:2][C:1]([OH:5])=[O:6]

参加物

4

反応物 2

HCID 72573,4-DichloroanilineHCID 18303beta-BUTYROLACTONE

生成物 1

HCID 2948103-(3,4-Dichloroanilino)butanoic acid収率 51.6%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

86 g (1.00 mole) of β-butyrolactone was added to 162 g (1.00 mole) of 3,4-dichloroaniline, and this mixture was stirred at 110°-120° C. for 1 hour and then allowed to cool to room temperature. To the resulting reaction solution was added 1000 ml of ether. This mixture was filtered to remove any insoluble matter, and the filtrate thus obtained was extracted with 750 ml of a 2N aqueous solution of sodium hydroxide. This extract was acidified with 130 ml of concentrated hydrochloric acid and then extracted with 1000 ml of ether. The ether layer was separated, dried over anhydrous sodium sulfate and then evaporated to dryness. Thus, there was obtained 128 g (51.6% yield) of 3-(3,4-dichloroanilino) butyric acid in the form of pale-yellow crystals.

後処理

  1. customTo the resulting reaction solution
  2. filtrationThis mixture was filtered
  3. customto remove any insoluble matter
  4. customthe filtrate thus obtained
  5. extractionwas extracted with 750 ml of a 2N aqueous solution of sodium hydroxide
  6. extractionextracted with 1000 ml of ether
  7. customThe ether layer was separated
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-f8942eeafac7400f808f4bac3742f7f3
出典データセット
uspto-grants-1988_01
特許番号
US04720495

関連ノート

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