تفاعل #91300

معادلة التفاعل

4′-(trifluoromethyl)-4-biphenylcarbaldehyde

N,N-diethylethylenediamine

→

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

المذيبات

toluene

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر