反応 #587218

ord-b381ecc26f9f428699735f10065d7368

反応条件

温度
22°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reactor was purged 3 times with 110 psig (8.60×105 Pa) of H2 at 22° C
  2. 2
    その他GC (conditions: 180° C./5 minutes/10° C.-minutes rate/270° C./RT=9.37 minutes)

実験手順

4,4′-Methylenebis(benzeneamine) (8.0 g, 40 mmol), acetone (10.0 g, 172 mmol), Pt(S)/C (0.5 g), and toluene (50.0g) were charged into reactor. The reactor was purged 3 times with 110 psig (8.60×105 Pa) of H2 at 22° C. The reaction mixture was then stirred at 22° C. under 110 psig (8.60×105 Pa) of H2 overnight. GC (conditions: 180° C./5 minutes/10° C.-minutes rate/270° C./RT=9.37 minutes) showed 100% conversion of 4,4′-methylenebis(benzeneamine), and a 98% yield of N,N′-diisopropyl-4,4′-methylenebis(benzeneamine). The structure of the product was confirmed by GC-MS. No tertiary diamine was detected either by GC or by GC-MS.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07767858B2uspto-grants-2010_08