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Methanol → Benzene-1,3,5-triyltrimethanamine

HRID 2166854
ノート
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反応式

HRID 2166854 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]>[Ni].[Cr].[OH-].[Na+].C1(C)C(C)=CC=CC=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

8

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 4

HCID 935Nickel触媒HCID 14798Sodium Hydroxide触媒
HCID 23976
Chromium
触媒
HCID 7237O-Xylene溶媒

実験手順

In a 300-ml capacity autoclave equipped with a magnetic stirrer was sealed 15 g of 1,3,5-tricyanobenzene (MTN), together with 15 g of Raney nickel.chromium catalyst (atomic ratio of Ni:Cr=49:1), 27 ml of methanol, 63 ml of xylene and 0.18 g of caustic soda. Hydrogen gas was fed into it at initial pressure of 100 kg/cm2G, and the reaction was carried out at 100° C., whereby 0.59 mole of hydrogen was absorbed for 35 minutes. The catalyst was filtered out, and the solvent was evaporated, followed by concentration under reduced pressure. By the above procedure, there was obtained 12.8 g of colorless crystals of 1,3,5-tris(aminomethyl)benzene (MTA). The substance showed melting point of 49° to 51° C. and boiling point of 136° to 139° C./0.4 mmHg.

後処理

  1. customIn a 300-ml capacity autoclave equipped with a magnetic stirrer
  2. customwas carried out at 100° C.
  3. filtrationThe catalyst was filtered out
  4. customthe solvent was evaporated
  5. concentrationfollowed by concentration under reduced pressure

出典と根拠

ORDレコード
ord-60f9779b8ece432e8d95499f6596120e
出典データセット
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04389519

反応ノート

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