Reaktion #91300

Reaktionsgleichung

4′-(trifluoromethyl)-4-biphenylcarbaldehyde

N,N-diethylethylenediamine

→

N,N-diethyl-N′-{[4′-(trifluoromethyl)-4-biphenylyl]methyl}-1,2-ethanediamine

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas hydrogenated at 20±3° C.
2. 2
   FiltrationThe reaction mixture was filtered
3. 3
   Waschenthe catalyst bed washed with toluene (2×36.7 kg)
4. 4
   WaschenThe solution was washed with water (84.8 kg)
5. 5
   Einengenconcentrated under reduced pressure to ca. 85 L
6. 6
   SonstigeThis concentrate was used in the next step, Example 6, without further purification

Vorschrift

A mixture of 4′-(trifluoromethyl)-4-biphenylcarbaldehyde, (43.6 kg, 1.1 eq., see WO 01/60805), N,N-diethylethylenediamine (21.2 kg, 1.15 equiv.) and 5% palladium on charcoal (Degussa E101 N/W, 50% wet paste, 1.7 kg) in toluene (138 Kg) was hydrogenated at 20±3° C. and 50 psi until completion. The reaction mixture was filtered and the catalyst bed washed with toluene (2×36.7 kg). The solution was washed with water (84.8 kg) and concentrated under reduced pressure to ca. 85 L. This concentrate was used in the next step, Example 6, without further purification.

Quelle