Hydrochloric Acid → 1-tert-Butyl-1H-pyrazole

HRID 57845

Reaktionsgleichung

Reaktionsgleichung von HRID 57845
CO[CH:3](OC)[CH2:4][CH:5](OC)OC.Cl.[C:13]([NH:17][NH2:18])([CH3:16])([CH3:15])[CH3:14].Cl.O>CCO>[C:13]([N:17]1[CH:5]=[CH:4][CH:3]=[N:18]1)([CH3:16])([CH3:15])[CH3:14]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 66019TetramethoxypropaneHCID 81889tert-Butylhydrazine monohydrochloride

Produkt 1

HCID 134698151-tert-Butyl-1H-pyrazoleAusbeute 89,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 1,1,3,3-tetramethoxypropane (3.7 g, 22.6 mmol), tert-butylhydrazine hydrochloride (2.8 g, 22.6 mmol), and conc. HCl (6 mL, 72 mmol) in EtOH (30 mL) was heated at reflux overnight. The reaction mixture was poured into water and the resulting mixture was extracted with ether (30 mL×3). The combined organics was washed with brine (20 mL), dried over MgSO4, and concentrated under reduced pressure to afford 1-tert-butyl-1H-pyrazole as a white solid (2.5 g, 89%). MS (ESI) m/z: 125 [M+H]+.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. extractionthe resulting mixture was extracted with ether (30 mL×3)
  4. washThe combined organics was washed with brine (20 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6a335cf3c39a4015825d004aca41beae
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434725B2

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