Hydrochloric Acid → 2-Amino-6-(4-aminophenyl)-6-methylheptane

HRID 2296370

Reaktionsgleichung

Cl.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.O[C:11]([CH3:19])([CH3:18])[CH2:12][CH2:13][CH2:14][CH:15]([NH2:17])[CH3:16].[OH-].[Na+]>[Cl-].[Zn+2].[Cl-].[Ta].O>[NH2:17][CH:15]([CH2:14][CH2:13][CH2:12][C:11]([C:6]1[CH:7]=[CH:8][C:3]([NH2:2])=[CH:4][CH:5]=1)([CH3:19])[CH3:18])[CH3:16]

Komponenten

Reaktionsbedingungen

Temperatur: 185 °C

Versuchsvorschrift

To a solution of 102 parts of anhydrous zinc chloride in 153 parts of 36% w/w aqueous hydrochloric acid and 200 parts of water are added 140 parts of aniline and 136 parts of 6-hydroxy-6-methyl-2-heptylamine hydrochloride (heptaminol hydrochloride). The whole is charged to a 1 liter tantalum-lined autoclave and stirred at 185° C. for 24 hours. The reaction mixture, after being discharged from the autoclave, is added to a hot solution of 750 parts sodium hydroxide in 1500 parts of water and stirred until cool. The organic phase is extracted with diethylether, washed with water, evaporated and distilled under reduced pressure. After recovering 58 parts of aniline there are obtained 135 parts of 2-amino-6-(4-amino-phenyl)-6-methyl-heptane boiling point 138°-40° C./65 Pa (82% yield based on heptaminol).

Aufarbeitung

stirringstirred
temperatureuntil cool
extractionThe organic phase is extracted with diethylether
washwashed with water
customevaporated
distillationdistilled under reduced pressure
customAfter recovering 58 parts of aniline

Quellen und Nachweise

ORD-Eintrag: ord-3e401ff2a45b426fa5a1c001b420fd1b
Quelldatensatz: uspto-grants-1984_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04429110

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