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Ammonia → 2-[3-(2-Aminoethyl)phenyl]ethanamine

HRID 1757481
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HRID 1757481 반응식
[C:1]1([CH2:10][C:11]#[N:12])[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]#[N:9])[CH:2]=1.N>[Ni].C(O)C>[NH2:9][CH2:8][CH2:7][C:3]1[CH:4]=[CH:5][CH:6]=[C:1]([CH2:10][CH2:11][NH2:12])[CH:2]=1
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참가 물질

5

반응물 2

HCID 222AmmoniaHCID 693751,3-Benzenediacetonitrile

생성물 1

HCID 27496402-[3-(2-Aminoethyl)phenyl]ethanamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

A mixture of 25.0 g (0.16 mmol) meta-xylylene dicyanide, 300 ml ethanol and50 ml conc. NH3 is hydrogenated in the presence of Raney nickel for 5 hrs. at 100° C. and 150 bar. One then filters off with suction and evaporates. The residue is dissolved in ether, the solution is clarified with active carbon and finally mixed with HCl-containing ether, whereby the dihydrochloride precipitates out. One filters off with suction, washeswith ether and dries. Yield 23.2 g (61% of theory) of dihydrochloride with the m.p. 282°-286° C.

후처리

  1. customat 100° C.
  2. customevaporates
  3. dissolutionThe residue is dissolved in ether
  4. additionfinally mixed with HCl-
  5. additioncontaining ether, whereby the dihydrochloride
  6. customprecipitates out

출처 및 근거

ORD 기록
ord-4f321a6bab234c8699274f46ff041bbd
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05446065

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