Ammonia → 2-Butyl-2-ethyl-1,5-pentanediamine

HRID 374365노트

반응식

HRID 374365 반응식
[CH2:1]([C:5]([CH2:12][CH3:13])([CH2:8][CH2:9][C:10]#[N:11])[CH:6]=O)[CH2:2][CH2:3][CH3:4].[NH3:14].O=[Si]=O.[H][H]>>[CH2:1]([C:5]1([CH2:12][CH3:13])[CH2:8][CH2:9][CH2:10][NH:11][CH2:6]1)[CH2:2][CH2:3][CH3:4].[CH2:1]([C:5]([CH2:12][CH3:13])([CH2:8][CH2:9][CH2:10][NH2:11])[CH2:6][NH2:14])[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 222Ammonia2회HCID 24261SilicaHCID 2205444-Ethyl-4-formyloctanenitrileHCID 178418361HCID 178418361, 화합물

생성물 2

HCID 49833442-Butyl-2-ethyl-1,5-pentanediamineHCID 149931223-Butyl-3-ethylpiperidine

실험 절차

41.6 g per hour of 2-butyl-2-ethyl-4-cyanobutanal (purity 90%, 37.4 g, 0.207 mol) and 1073 ml (646 g, 38.0 mol) per hour of liquid ammonia were pumped at 250 bar and 50° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) upstream of the hydrogenation reactor and filled with 43.3 g (96 ml) of a Y-zeolite pelleted with Aerosil 200 (HY-zeolite: Aerosil 200 =9:1, SiO2 :Al2O3 =6:1). The product stream was subsequently passed through the hydrogenation reactor from bottom to top at 250 bar and 120° C. while simultaneously passing 80 l(S.T.P.)/h (3.6 mol) of hydrogen through the reactor. The product stream was decompressed to atmospheric pressure and NH3 was removed by distillation. The product from 34.1 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 358.3 g of 3-butyl-3-ethylpiperidine and 747.7 g of 2-butyl-2-ethylpentane-1,5-diamine. The diamine yield was 56.9% of theory.

후처리

  1. temperature(diameter 16 mm, fill level 50 cm, oil-heated twin jacket) upstream of the hydrogenation reactor
  2. customto top at 250 bar and 120° C.
  3. customwas removed by distillation
  4. customThe product from 34.1 hours was separated by fractional distillation on a 30 cm

출처 및 근거

ORD 기록
ord-98e773336d114745b17a57dceb1dab03
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166443

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