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Methanol → Benzene-1,3,5-triyltrimethanamine

HRID 435182
ノート
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反応式

HRID 435182 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.[H][H]>[Cr].[Ni].[OH-].[Na+].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 3

HCID 887MethanolHCID 82587Benzene-1,3,5-tricarbonitrileHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 10989469Benzene-1,3,5-triyltrimethanamine収率 79.1%

試薬・触媒・溶媒 3

HCID 14798Sodium Hydroxide触媒HCID 11320920Chromium 22, nickel 78 (atomic)
触媒
HCID 7929M-Xylene溶媒

実験手順

15 g of 1,3,5-tricyanobenzene (MTN) was charged into a magnetically stirring type autoclave having a 300 ml capacity together with 15 g of Raney nickel-chromium catalyst (atomic ratio: Ni:Cr=49:1), 27 ml of methanol, 63 ml of m-xylene and 0.18 g of sodium hydroxide. Hydrogen was injected thereinto under an initial pressure of 100 kg/cm2G and reaction was effected at 100° C. to cause absorption of 0.59 mole of hydrogen for 35 minutes. The catalyst was filtered off and the solvent was distilled out. Then, distillation under reduced pressure was effected to obtain 12.8 g of colorless crystal of 1,3,5-tris(aminomethyl) benzene (MTA). The product had a melting point of 49° to 51° C. and a boiling point of 136° to 139° C./0.4 mmHg.

後処理

  1. customunder an initial pressure of 100 kg/cm2G and reaction
  2. customwas effected at 100° C.
  3. filtrationThe catalyst was filtered off
  4. distillationthe solvent was distilled out
  5. distillationThen, distillation under reduced pressure

出典と根拠

ORDレコード
ord-014d674616124c7d96927af8ee7eaebc
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04400525

反応ノート

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