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Diglycolamine → 4-Chloro-2-(beta-hydroxyethoxyethyl)amino-6-(beta-hydroxyethoxyethyl)aminonitrobenzene

HRID 231377
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인쇄 미리보기

반응식

HRID 231377 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].[NH2:13][CH2:14][CH2:15][O:16][CH2:17][CH2:18][OH:19]>O1CCOCC1>[Cl:8][C:6]1[CH:5]=[C:4]([NH:13][CH2:14][CH2:15][O:16][CH2:17][CH2:18][OH:19])[C:3]([N+:10]([O-:12])=[O:11])=[C:2]([NH:13][CH2:14][CH2:15][O:16][CH2:17][CH2:18][OH:19])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 13578DiglycolamineHCID 292282,4,6-Trichloronitrobenzene

생성물 1

HCID 200710944-Chloro-2-(beta-hydroxyethoxyethyl)amino-6-(beta-hydroxyethoxyethyl)aminonitrobenzene

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

The mixture consisting of 0.1 mole (22.6 g) of 2,4,6-trichloronitrobenzene, 0.6 mole (63 g) of 2-(β-aminoethoxy)ethanol and 20 ml of dioxan is heated to reflux of the dioxon. After 4 hours, the reaction mixture is poured onto to 200 g of ice. The product expected crystallizes on acidifying with concentrated hydrochloric acid. After draining, washing with water and drying by heating under vacuum, the product is recrystallized from acetonitrile and then from toluene. It melts at 83° C.

후처리

  1. temperatureis heated
  2. temperatureto reflux of the dioxon
  3. customThe product expected crystallizes
  4. washwashing with water
  5. customdrying
  6. temperatureby heating under vacuum
  7. customthe product is recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-4e26d05449f846529a1c30fbcf8ff566
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04845293

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