反応 #3855

ord-cd6c544d691047e28572b2af8207df9c

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After two hours the reaction mixture was cooled
  2. 2
    ろ過filtered
  3. 3
    その他to remove the catalyst
  4. 4
    その他to give 205.3 g of water-white clear liquid which
  5. 5
    workup.DISTILLATIONwas fractionally distilled under reduced pressure
  6. 6
    その他The desired product recovered
  7. 7
    その他a boiling point (b.p.) of 62°-64° C./0.15 mm Hg

実験手順

A mixture of 146 g (1.1 moles) of N-(2-amino-2-methylpropyl)-1,2-ethanediamine, 84.4 (1.17 moles) of 2-butanone, 300 ml methanol, and 3.0 g of 10% platinum on carbon were reacted in a 1 liter autoclave at 80° C. under 800 pounds per square inch (psi) hydrogen pressure. After two hours the reaction mixture was cooled, then filtered to remove the catalyst. The filtrate was stripped to give 205.3 g of water-white clear liquid which was fractionally distilled under reduced pressure. The desired product recovered was found to weigh 144.5 g (69.5% yield), and has a boiling point (b.p.) of 62°-64° C./0.15 mm Hg.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04722806uspto-grants-1988_02