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

HRID 231376
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HRID 231376 반응식
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
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참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 292282,4,6-Trichloronitrobenzene

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
10 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-7fe7cdb41be94795b36ccba555bb7f17
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04845293

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