反応 #94107

ord-91367ad1c6eb45eeb010593806d03789

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The product crystallises out at room temperature
  2. 2
    workup.DISSOLUTIONis dissolved
  3. 3
    workup.ADDITIONby boiling with the addition of a further 650 ml of isopropanol
  4. 4
    ろ過The catalyst is filtered off
  5. 5
    その他N,N'-bis-(2-hydroxybenzyl)hexamethylenediamine crystallises out
  6. 6
    温度on cooling

実験手順

122.1 g of a bisazomethine prepared from 2 mols of salicylaldehyde and 1 mol of hexamethylenediamine and having a melting point of 72°-73° C. are hydrogenated in 550 ml of isopropanol in an autoclave in the presence of 8 g of Raney nickel at 75° C. and under a pressure of 90 atmospheres. The product crystallises out at room temperature and is dissolved by boiling with the addition of a further 650 ml of isopropanol. The catalyst is filtered off, and N,N'-bis-(2-hydroxybenzyl)hexamethylenediamine crystallises out on cooling.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04129556uspto-grants-1978_12