Ammonia → 3,3-Dimethylpiperidine

HRID 374360노트

반응식

HRID 374360 반응식
[CH3:1][C:2]([CH3:9])([CH2:5][CH2:6][C:7]#[N:8])[CH:3]=O.[NH3:10].[H][H]>>[CH3:1][C:2]1([CH3:9])[CH2:5][CH2:6][CH2:7][NH:8][CH2:3]1.[CH3:1][C:2]([CH3:9])([CH2:5][CH2:6][CH2:7][NH2:8])[CH2:3][NH2:10]

참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 802314-Formyl-4-methylvaleronitrileHCID 178418361HCID 178418361, 화합물

생성물 2

HCID 709423,3-DimethylpiperidineHCID 110407352,2-Dimethylpentane-1,5-diamine

실험 절차

34.0 g per hour of 2,2-dimethyl-4-cyanobutanal (purity 93.4%, 31.8 g, 0.254 mol) and 1450 ml (870 g, 51.1 mol) per hour of liquid ammonia were pumped at 250 bar and 60° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) upstream of the hydrogenation reactor and filled with 63.5 g (100 ml) of TiO2 (anatase) in the form of 1.5 mm pellets. The discharge from the reactor 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 32.4 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 344.8 g of 3,3-dimethylpiperidine (b.p. 50°-52° C./210 mmHg) and 753.6 g of 2,2-dimethylpentane-1,5-diamine (b.p.=72° C./8 mmHg). The diamine yield was 70.5% 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 32.4 hours was separated by fractional distillation on a 30 cm

출처 및 근거

ORD 기록
ord-5b53f5c3534b4e5e9d0ff2f92a8ce4db
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166443

반응 노트

불러오는 중…