3-Cyano-4-isobutoxyaniline hydrochloride → 3-Cyano-4-isobutoxy-phenylhydrazine

HRID 850063Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 850063
Cl.[C:2]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][CH:13]([CH3:15])[CH3:14])[NH2:7])#[N:3].[N:16]([O-])=O.[Na+]>>[C:2]([C:4]1[CH:5]=[C:6]([NH:7][NH2:16])[CH:8]=[CH:9][C:10]=1[O:11][CH2:12][CH:13]([CH3:15])[CH3:14])#[N:3]

Komponenten

3

Edukt 2

HCID 193660273-Cyano-4-isobutoxyaniline hydrochlorideHCID 23668193Sodium Nitrite

Produkt 1

HCID 154065483-Cyano-4-isobutoxy-phenylhydrazineAusbeute 82,8 %

Versuchsvorschrift

To an aqueous solution (34 ml) of 3-cyano-4-isobutoxyaniline hydrochloride (20 g) were added sodium nitrite (6.8 g), stannous chloride dihydrate (61 g) and con. hydrochloric add (100 ml) with stirring under ice-cooling. After the completion of the reaction, precipitated crystals were collected by filtration. The crystals were added to water, and the mixture was neutralized with aqueous sodium hydroxide solution, extracted with a mixed solvent of toluene and tert-butanol, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 15 g of 3-cyano-4-isobutoxy-phenylhydrazine.

Aufarbeitung

  1. additionhydrochloric add (100 ml)
  2. temperaturecooling
  3. customAfter the completion of the reaction
  4. customprecipitated crystals
  5. filtrationwere collected by filtration
  6. additionThe crystals were added to water
  7. extractionextracted with a mixed solvent of toluene and tert-butanol
  8. washwashed with water
  9. dry with materialdried over magnesium sulfate
  10. customThe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7930b7ff2d62446faaf6dfcd2c408bfc
Quelldatensatz
uspto-grants-2000_01
Patentnummer
US06015829

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