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Methanol → Benzene-1,3,5-triyltrimethanamine

HRID 1462885
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HRID 1462885 반응식
[C:1]([C:3]1[CH:8]=[C:7]([C:9]#[N:10])[CH:6]=[C:5]([C:11]#[N:12])[CH:4]=1)#[N:2].CO.[OH-].[Na+].[H][H]>[Cr].[Ni].C1(C)C=CC=C(C)C=1>[NH2:2][CH2:1][C:3]1[CH:4]=[C:5]([CH2:11][NH2:12])[CH:6]=[C:7]([CH2:9][NH2:10])[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 82587Benzene-1,3,5-tricarbonitrileHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 10989469Benzene-1,3,5-triyltrimethanamine수율 81%

시약·촉매·용매 2

HCID 11320920Chromium 22, nickel 78 (atomic)촉매
HCID 7929M-Xylene용매

실험 절차

1000 g of 1,3,5-tricyanobenzene (MTN) was charged in an autoclave having a 20 l capacity together with 400 g of Raney nickel-chromium catalyst (atomic ratio Ni:Cr=49:1), 1800 ml of methanol, 4.2 l of m-xylene and 32.6 g of sodium hydroxide. Hydrogen was injected thereinto under an initial pressure of 140 kg/cm2G and reaction was effected at 60°-102° C. to cause absorption of nearly theoretical amount of hydrogen for 31 minutes. The catalyst was filtered off and the solvent was distilled out. Then, distillation under reduced pressure was effected to obtain 874 g of colorless crystal of 1,3,5-tris(aminomethyl)benzene (MTA). The product had a melting point of 49°-51° C. and a boiling point of 136°-139° C./0.4 mmHg.

후처리

  1. customunder an initial pressure of 140 kg/cm2G and reaction
  2. customwas effected at 60°-102° C.
  3. customabsorption of nearly theoretical amount of hydrogen for 31 minutes
  4. filtrationThe catalyst was filtered off
  5. distillationthe solvent was distilled out
  6. distillationThen, distillation under reduced pressure

출처 및 근거

ORD 기록
ord-09e6397581c54340be9a6e012e99f8a1
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04461878

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