Reaktion #40375

ord-d40536500a4f4ac6b14cb0966f32001e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted three times with diethyl ether
  2. 2
    WaschenThe combined organic phases are washed with water
  3. 3
    Trocknendried with sodium sulfate
  4. 4
    SonstigeTo prepare the hydrochloride
  5. 5
    SonstigeThe solid precipitated
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigedried

Vorschrift

16.3 g (74 mmol) of N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide and 8.0 g of potassium hydroxide are refluxed for 15 hours in 60 mL ethylene glycol. The reaction mixture is combined with ice water and extracted three times with diethyl ether. The combined organic phases are washed with water, dried with sodium sulfate, and freed from solvent. To prepare the hydrochloride, the crude product is dissolved in acetonitrile and ethereal hydrochloric acid and diethyl ether are added successively. The solid precipitated is suction filtered and dried. Yield: 11.0 g (69%, hydrochloride); melting point 165° C.-167° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727984B2uspto-grants-2010_06