Methane → 1,5-Diaminonaphthalene

HRID 2399094

反応式

HRID 2399094 の反応式
[N+:1]([C:4]1[C:13]2[C:8](=[C:9]([N+:14]([O-])=O)[CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1)([O-])=O.O.C.[H][H]>NC1C=CC=CC=1.[Pt]>[NH2:1][C:4]1[C:13]2[C:8](=[C:9]([NH2:14])[CH:10]=[CH:11][CH:12]=2)[CH:7]=[CH:6][CH:5]=1

参加物

7

反応物 4

HCID 297MethaneHCID 962WaterHCID 118031,5-DinitronaphthaleneHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 167201,5-Diaminonaphthalene

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 6115Aniline溶媒

反応条件

温度
18 °C

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.

後処理

  1. customwas carried out at 50° C.
  2. customThe catalyst was separated off by filtration at 80° C.
  3. customthe aniline subsequently removed by water-vapour distillation
  4. filtrationthe precipitated crystallate filtered off
  5. customdried

出典と根拠

ORDレコード
ord-6f8e577bf58b4df1b0f9a6d6da3b45e1
出典データセット
uspto-grants-1977_05
特許番号
US04026944

関連ノート

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