Di-(2-nitroisobutyl)amine → Bis(2-amino-2-methylpropyl)amine

HRID 2215367

反応式

HRID 2215367 の反応式
[CH3:1][C:2]([N+:13]([O-])=O)([CH3:12])[CH2:3][NH:4][CH2:5][C:6]([N+:9]([O-])=O)([CH3:8])[CH3:7]>CO.[Ni]>[CH3:8][C:6]([NH2:9])([CH3:7])[CH2:5][NH:4][CH2:3][C:2]([NH2:13])([CH3:1])[CH3:12]

参加物

4

反応物 1

HCID 21951119Di-(2-nitroisobutyl)amine

生成物 1

HCID 226845Bis(2-amino-2-methylpropyl)amine

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

490 g (2.23 mol) of bis-(2-methyl-2-nitropropyl)amine from reaction 1) are dissolved in 1200 ml of methanol and transferred into an autoclave. 60 g of Raney Ni are added. The autoclave is closed and purged with nitrogen. Then, hydrogen is added until the hydrogen pressure is 50 bars. That pressure is maintained at room temperature for 8 hours and, subsequently, the reaction mixture is heated to 50° C. at the same pressure. The catalyst is then separated off by filtration and the mixture is distilled under vacuum (100° C./33.3 mbar). A colourless oil is recovered (Boiling point: 110° C./5 mbar).

後処理

  1. customThe autoclave is closed
  2. custompurged with nitrogen
  3. additionThen, hydrogen is added until the hydrogen pressure
  4. temperaturesubsequently, the reaction mixture is heated to 50° C. at the same pressure
  5. customThe catalyst is then separated off by filtration
  6. distillationthe mixture is distilled under vacuum (100° C./33.3 mbar)
  7. customA colourless oil is recovered (Boiling point: 110° C./5 mbar)

出典と根拠

ORDレコード
ord-9b5c2fefa2bd4c11bc70d34013b34e69
出典データセット
uspto-grants-2006_09
特許番号
US07109259B2

関連ノート

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