tert-Butylhydrazine → 1-tert-Butyl-3-methyl-1H-pyrazol-5-amine

HRID 1250419

Reaktionsgleichung

Reaktionsgleichung von HRID 1250419
[NH2:1]/[C:2](/[CH3:6])=[CH:3]\[C:4]#[N:5].[C:7]([NH:11]N)([CH3:10])([CH3:9])[CH3:8]>C(O)CCCC.C(OC(C)C)(C)C>[NH2:5][C:4]1[N:11]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:1]=[C:2]([CH3:6])[CH:3]=1

Komponenten

5

Edukt 2

HCID 81890tert-ButylhydrazineHCID 5325263(2Z)-3-Amino-2-butenenitrile

Produkt 1

HCID 7372001-tert-Butyl-3-methyl-1H-pyrazol-5-amineAusbeute 58,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 62761-PentanolLösungsmittelHCID 7914Diisopropyl EtherLösungsmittel

Versuchsvorschrift

To a solution of 16.4 g (0.2 mol) of 3-aminocrotononitrile in 100 cm3 of n-pentanol were added 19.4 g (0.22 mol) of tert-butylhydrazine. This solution was heated at reflux for 20 hours. The n-pentanol was subsequently distilled off under reduced pressure. A pale yellow solid was obtained, which was taken up in 100 cm3 of isopropyl ether at room temperature and filtered on a sinter funnel. After drying under vacuum at 40° C., 18 g of the expected product were obtained in the form of a pale yellow solid, the melting point of which was from 172 to 175° C.

Aufarbeitung

  1. temperatureThis solution was heated
  2. temperatureat reflux for 20 hours
  3. distillationThe n-pentanol was subsequently distilled off under reduced pressure
  4. customA pale yellow solid was obtained
  5. filtrationfiltered on a sinter funnel
  6. customAfter drying under vacuum at 40° C.

Quellen und Nachweise

ORD-Eintrag
ord-df24e070ab4641a5936b1a2d95fc29d4
Quelldatensatz
uspto-grants-2002_01
Patentnummer
US06338741B1

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