反応 #2486276

ord-6f8e577bf58b4df1b0f9a6d6da3b45e1

溶媒

反応条件

温度
18°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was carried out at 50° C.
  2. 2
    その他The catalyst was separated off by filtration at 80° C.
  3. 3
    その他the aniline subsequently removed by water-vapour distillation
  4. 4
    ろ過the precipitated crystallate filtered off
  5. 5
    その他dried

実験手順

60 g (0.275 mol) of 1,5-dinitro naphthalene were suspended, in a 700 ml stirrer autoclave, in 340 ml of aniline and treated with 18 g of water-moist, 1%-strength catalyst of platinum and activated charcoal corresponding to 8 g of dry catalyst. Hydrogenation was carried out at 50° C. and a hydrogen pressure of 10 bars, as was described in Example 1. The hydrogen uptake was finished after 2 hours. The catalyst was separated off by filtration at 80° C. and the aniline subsequently removed by water-vapour distillation. The distillation residue was cooled to 18° C. and the precipitated crystallate filtered off and dried. In this way 40 g (92% of the theory) of 1,5-diamino naphthalene of m.p. 188°-189° C. were obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04026944uspto-grants-1977_05