HCID 135428345, Verbindung → 1,4-Bis(alpha-aminobenzyl)benzene

HRID 442250Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 442250
[C:1](=[N:23]O)([C:8]1[CH:13]=[CH:12][C:11]([C:14](=[N:21]O)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H][H]>C(O)C.N.[Ni]>[NH2:21][CH:14]([C:11]1[CH:12]=[CH:13][C:8]([CH:1]([NH2:23])[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:9][CH:10]=1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

Komponenten

6

Edukt 2

HCID 135428345HCID 135428345, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 203406881,4-Bis(alpha-aminobenzyl)benzene

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 935NickelKatalysatorHCID 222AmmoniaLösungsmittelHCID 702EthanolLösungsmittel

Versuchsvorschrift

The dioxime from Step 2 (30 g) is dissolved in ethyl alcohol (300 ml), saturated with ammonia gas and Raney nickel catalyst W-6 (2 g) added. The mixture is subjected to 700 psi hydrogen pressure and heated at 70° for 3 hours. The catalyst is removed by filtration and 220 ml of ethanol is removed by distillation. The pale yellow precipitate is filtered and dried. Yield 28 g (91% of theory) mp 123°-127°. Calculated for C20H20N2 : C, 83.29%; H, 6.99%; N, 9.71%. Found: C, 83.07%; H, 6.89%; N, 9.59%.

Aufarbeitung

  1. addition(2 g) added
  2. temperatureheated at 70° for 3 hours
  3. customThe catalyst is removed by filtration and 220 ml of ethanol
  4. customis removed by distillation
  5. filtrationThe pale yellow precipitate is filtered
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ca8cb2545fd041d689b76e86656033b1
Quelldatensatz
uspto-grants-1977_08
Patentnummer
US04044139

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