1,4-Dicyanobenzene → 1,4-Benzenedimethanamine

HRID 1074305

Reaktionsgleichung

[C:1](#[N:10])[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.C(O)C.N>[Ni]>[C:2]1([CH2:1][NH2:10])[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 150 °C

Versuchsvorschrift

5.1 g of terephthalonitrile, 1.0 g of catalyst (Ni 5136P from Harshaw/Filtrol--contains 65% nickel on a silica-alumina support), and about 85 g of ethanol/ammonia (contains about 10 wt % ammonia) were charged to a 300 cc stainless steel pressure reactor. After a nitrogen purge, the vessel was charged to a pressure of 500 to 1000 psi with hydrogen. The temperature was then increased until the reaction temperature of 150° C. had been obtained (typically 20-30 min). After the desired reaction interval, the contents were cooled and sampled. Product analysis and conversion were determined by gas chromatography. Yields of para-xylylenediamine varied between 63-81% depending on hydrogen pressure and reaction time which is preferrably from 2 to 8 hours. The remainder of the product was saturated para-xylylenediamine (1.4 bis (aminomethyl) cyclohexane. Table IV sets forth specific examples of reactions run to obtain the diamines from hydrogenation of terephthalonitrile.

Aufarbeitung

additionwere charged to a 300 cc stainless steel pressure reactor
customAfter a nitrogen purge
additionthe vessel was charged to a pressure of 500 to 1000 psi with hydrogen
customhad been obtained (typically 20-30 min)
customAfter the desired reaction interval
temperaturethe contents were cooled
aliquotsampled

Quellen und Nachweise

ORD-Eintrag: ord-fba17c8fe9b94c5db4df0ed9545d6aba
Quelldatensatz: uspto-grants-1990_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04973746

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