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Methanol → Benzene-1,3,5-triyltrimethanamine

HRID 1462885
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1462885
[C:1]([C:3]1[CH:8]=[C:7]([C:9]#[N:10])[CH:6]=[C:5]([C:11]#[N:12])[CH:4]=1)#[N:2].CO.[OH-].[Na+].[H][H]>[Cr].[Ni].C1(C)C=CC=C(C)C=1>[NH2:2][CH2:1][C:3]1[CH:4]=[C:5]([CH2:11][NH2:12])[CH:6]=[C:7]([CH2:9][NH2:10])[CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 82587Benzene-1,3,5-tricarbonitrileHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 10989469Benzene-1,3,5-triyltrimethanamineAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 11320920
Chromium 22, nickel 78 (atomic)
Katalysator
HCID 7929M-XyleneLösungsmittel

Versuchsvorschrift

1000 g of 1,3,5-tricyanobenzene (MTN) was charged in an autoclave having a 20 l capacity together with 400 g of Raney nickel-chromium catalyst (atomic ratio Ni:Cr=49:1), 1800 ml of methanol, 4.2 l of m-xylene and 32.6 g of sodium hydroxide. Hydrogen was injected thereinto under an initial pressure of 140 kg/cm2G and reaction was effected at 60°-102° C. to cause absorption of nearly theoretical amount of hydrogen for 31 minutes. The catalyst was filtered off and the solvent was distilled out. Then, distillation under reduced pressure was effected to obtain 874 g of colorless crystal of 1,3,5-tris(aminomethyl)benzene (MTA). The product had a melting point of 49°-51° C. and a boiling point of 136°-139° C./0.4 mmHg.

Aufarbeitung

  1. customunder an initial pressure of 140 kg/cm2G and reaction
  2. customwas effected at 60°-102° C.
  3. customabsorption of nearly theoretical amount of hydrogen for 31 minutes
  4. filtrationThe catalyst was filtered off
  5. distillationthe solvent was distilled out
  6. distillationThen, distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-09e6397581c54340be9a6e012e99f8a1
Quelldatensatz
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04461878

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