Ammonia → 4,4-Dimethyl-1,5-hexanediamine

HRID 2225963

반응식

HRID 2225963 반응식
[CH3:1][C:2]([CH3:10])([C:7](=O)[CH3:8])[CH2:3][CH2:4][C:5]#[N:6].N.CC1C(C)(C)CCC[NH:14]1>[O-2].[O-2].[Ti+4].[H][H]>[CH3:1][C:2]([CH3:10])([CH:7]([NH2:14])[CH3:8])[CH2:3][CH2:4][CH2:5][NH2:6]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 131577824,4-Dimethyl-5-oxohexanenitrileHCID 190051912,3,3-Trimethylpiperidine

생성물 1

HCID 183143544,4-Dimethyl-1,5-hexanediamine수율 93%

시약·촉매·용매 2

HCID 162651Titanium oxide (Ti3O)촉매HCID 178418361HCID 178418361, 화합물용매

실험 절차

10 g of 4,4,-dimethyl-5-oxohexanenitrile (purity 97.2%) and 195 g of liquid ammonia were pumped hourly from bottom to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) arranged before the hydrogenation reactor and filled with 63.5 g (100 ml) of titanium dioxide (anatase) in the form of 1.5 mm pellets. 100 l (s.t.p.)/h of hydrogen were subsequently passed in, and the product discharged from the upstream imination reactor was passed through the hydrogenation reactor from bottom to top at 250 bar and 110° C. The mixture was decompressed to atmospheric pressure, the ammonia was removed by distillation, and the hydrogenation product was analyzed quantitatively by means of gas chromatography, giving a yield of 93.0% of 4,4-dimethyl-1,5-hexanediamine and 4.5% of 2,3,3-trimethylpiperidine.

후처리

  1. customto top at 250 bar and 80° C. through a tubular reactor
  2. temperature(diameter 16 mm, fill level 50 cm, oil-heated twin jacket)
  3. customto top at 250 bar and 110° C
  4. customthe ammonia was removed by distillation

출처 및 근거

ORD 기록
ord-7bcfdf88c3ee4646af86ea7d7bde11eb
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344983

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