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Hydrochloric Acid → 2-[(4-phenyl-4H-1,2,4-triazol-3-yl)sulfanyl]acetic acid

HRID 1421206
ノート
印刷プレビュー

反応式

HRID 1421206 の反応式
[C:1]1([N:7]2[CH:11]=[N:10][N:9]=[C:8]2[SH:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:14][C:15]([O-:17])=[O:16].[Na+].[OH-].[Na+].Cl>O.C(O)C>[C:15]([CH2:14][S:12][C:8]1[N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:11]=[N:10][N:9]=1)([OH:17])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23665759Sodium chloroacetateHCID 178527969HCID 178527969、化合物

生成物 1

HCID 7157412-[(4-phenyl-4H-1,2,4-triazol-3-yl)sulfanyl]acetic acid収率 46.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

Into 500 ml of ethanol were suspended 53 g (0.3 mol) of 4-phenyl-3-mercapto-1,2,4-triazole and 44.1 g (0.36 mol) of sodium chloroacetate. Thereto was added an aqueous solution prepared by dissolving 15.5 g (0.36 mol) of sodium hydroxide (purity, 93%) into 60 ml of water. This mixture was kept at 50° C. for 3 hours to-react the reactants. The reaction mixture was allowed to cool to room temperature, neutralized by dropwise adding 31 ml (0.36 mol) of concentrated hydrochloric acid, and then cooled to 10° C. or lower with ice. The resulting precipitate was taken out by filtration. To the precipitate was added 1.5 l of ethanol. This mixture was heated, and the insoluble matter was taken out by filtration. Thereafter recrystallization was conducted with cooling to obtain 32.3 g (0.14 mol) of the desired mercaptoacetic acid derivative. Yield, 45.8%.

後処理

  1. additionThereto was added an aqueous solution
  2. customprepared
  3. customto-react the reactants
  4. temperaturecooled to 10° C. or lower with ice
  5. filtrationThe resulting precipitate was taken out by filtration
  6. additionTo the precipitate was added 1.5 l of ethanol
  7. temperatureThis mixture was heated
  8. filtrationthe insoluble matter was taken out by filtration
  9. customThereafter recrystallization
  10. temperaturewith cooling

出典と根拠

ORDレコード
ord-4a4e97962106484a857fd0c75859f0a5
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06074813

反応ノート

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