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Ethylenediamine → 4-Chloro-2-(beta-aminoethyl)amino-6-(beta-aminoethyl)aminonitrobenzene

HRID 231376
ノート
印刷プレビュー

反応式

HRID 231376 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[C:3]=1[N+:10]([O-:12])=[O:11].[CH2:13]([NH2:16])[CH2:14][NH2:15]>O1CCOCC1>[Cl:8][C:6]1[CH:5]=[C:4]([NH:15][CH2:14][CH2:13][NH2:16])[C:3]([N+:10]([O-:12])=[O:11])=[C:2]([NH:15][CH2:14][CH2:13][NH2:16])[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 292282,4,6-Trichloronitrobenzene

生成物 1

HCID 200352444-Chloro-2-(beta-aminoethyl)amino-6-(beta-aminoethyl)aminonitrobenzene

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
10 °C

実験手順

0.35 mole (79 g) of 2,4,6-trichloronitrobenzene is added to 280 ml of ethylenediamine diluted with 140 ml of dioxan, the temperature being maintained at 10° C. The mixture is heated for 2 hours at 50° C. The product expected precipitates on standing overnight at ambient temperature. After draining and re-impasting in water, the product is recrystallized from isopropanol in order to remove an insoluble product by filtering in the heated state. After drying under reduced pressure in the presence of phosphorous pentoxide, it melts at 113° C.

後処理

  1. temperatureThe mixture is heated for 2 hours at 50° C
  2. customThe product expected precipitates
  3. customthe product is recrystallized from isopropanol in order
  4. customto remove an insoluble product
  5. filtrationby filtering in the heated state
  6. dry with materialAfter drying under reduced pressure in the presence of phosphorous pentoxide, it melts at 113° C.

出典と根拠

ORDレコード
ord-7fe7cdb41be94795b36ccba555bb7f17
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04845293

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート