Sulfuric Acid → Ethyl 2-[2-(3,5-dichlorophenyl)hydrazinylidene]propanoate

HRID 568184

Reaktionsgleichung

Reaktionsgleichung von HRID 568184
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH2:10])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[C:11]([O:16][CH2:17][CH3:18])(=[O:15])[C:12]([CH3:14])=O.S(=O)(=O)(O)O.C(=O)(O)[O-].[Na+]>O.C(OCC)(=O)C.C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][N:10]=[C:12]([CH3:14])[C:11]([O:16][CH2:17][CH3:18])=[O:15])[CH:5]=[C:6]([Cl:8])[CH:7]=1

Komponenten

8

Edukt 4

HCID 1118Sulfuric AcidHCID 12041Ethyl pyruvateHCID 516892Sodium BicarbonateHCID 6004693,5-Dichlorophenylhydrazine

Produkt 1

HCID 71333082Ethyl 2-[2-(3,5-dichlorophenyl)hydrazinylidene]propanoate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Combine 3,5-dichlorophenylhydrazine (300 g) and ethanol (2 L). Add ethyl pyruvate (153.6 mL) and sulfuric acid (25 mL). After 3 hours, evaporate in vacuo to obtain a residue. Cover the residue with ethyl acetate and water. Add solid sodium bicarbonate until the aqueous layer is neutralized. Separate the layers and extract the aqueous layer with ethyl acetate. Combine the organic layers, dry over MgSO4, filter, and evaporate in vacuo to give ethyl pyruvate-3,5-dichlorophenylhydrazone.

Aufarbeitung

  1. customevaporate in vacuo
  2. customto obtain a residue
  3. customSeparate the layers
  4. extractionextract the aqueous layer with ethyl acetate
  5. dry with materialdry over MgSO4
  6. filtrationfilter
  7. customevaporate in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-cbc1d41875ea43ab9b0395657970d370
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06180786B2

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