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Ammonia → 2-Methyl-2-propylpentane-1,5-diamine

HRID 374362
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HRID 374362 반응식
[CH3:1][C:2]([CH2:9][CH2:10][CH3:11])([CH2:5][CH2:6][C:7]#[N:8])[CH:3]=O.[NH3:12].[H][H]>>[CH3:1][C:2]1([CH2:9][CH2:10][CH3:11])[CH2:5][CH2:6][CH2:7][NH:8][CH2:3]1.[CH3:1][C:2]([CH2:9][CH2:10][CH3:11])([CH2:5][CH2:6][CH2:7][NH2:8])[CH2:3][NH2:12]
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참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 149931194-Formyl-4-methylheptanenitrileHCID 178418361HCID 178418361, 화합물

생성물 2

HCID 149931202-Methyl-2-propylpentane-1,5-diamineHCID 149931213-Methyl-3-propylpiperidine

실험 절차

Example 2 was repeated, with 55.9 g of 2-methyl-2-propyl-4-cyanobutanal (purity 86.6%, 48.4 g, 0.316 mol) per hour and 1365 ml (819 g, 48.2 mol) per hour of liquid ammonia at 250 bar and 60° C. being pumped through the imination reactor. The product stream was subsequently passed through the hydrogenation reactor from bottom to top at 250 bar and 120° C. while simultaneously passing 100 l(S.T.P.)/h (4.5 mol) of hydrogen through the reactor. The product stream was decompressed to atmospheric pressure and NH3 was removed by distillation. The product from 16.8 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 174.4 g of 3-methyl-3-propylpiperidine and 501.6 g of 2-methyl-2-propylpentane-1,5-diamine. The diamine yield was 59.6% of theory.

후처리

  1. customto top at 250 bar and 120° C.
  2. customwas removed by distillation
  3. customThe product from 16.8 hours was separated by fractional distillation on a 30 cm

출처 및 근거

ORD 기록
ord-4b99f27123164efab4e8e10886dedd4a
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05166443

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