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

HRID 2215367

반응식

HRID 2215367 반응식
[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]

참가 물질

4

반응물 1

HCID 21951119Di-(2-nitroisobutyl)amine

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-9b5c2fefa2bd4c11bc70d34013b34e69
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07109259B2

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