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Methanol → Benzene-1,3,5-triyltrimethanamine

HRID 1462885
ノート
印刷プレビュー

反応式

HRID 1462885 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 82587Benzene-1,3,5-tricarbonitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 10989469Benzene-1,3,5-triyltrimethanamine収率 81%

試薬・触媒・溶媒 2

HCID 11320920Chromium 22, nickel 78 (atomic)触媒
HCID 7929
M-Xylene
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09e6397581c54340be9a6e012e99f8a1
出典データセット
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04461878

反応ノート

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