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2,4,6-Trichloronitrobenzene → 4-Chloro-2-(beta-diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene

HRID 981822
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인쇄 미리보기

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HRID 981822 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]([N:15]([CH2:19][CH3:20])[CH2:16][CH2:17][NH2:18])[CH3:14]>O>[Cl:8][C:6]1[CH:5]=[C:4]([NH:18][CH2:17][CH2:16][N:15]([CH2:19][CH3:20])[CH2:13][CH3:14])[C:3]([N+:10]([O-:12])=[O:11])=[C:2]([NH:18][CH2:17][CH2:16][N:15]([CH2:19][CH3:20])[CH2:13][CH3:14])[CH:7]=1
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참가 물질

4

반응물 2

HCID 292282,4,6-TrichloronitrobenzeneHCID 60993N,N-Diethylethylenediamine

생성물 1

HCID 200710864-Chloro-2-(beta-diethylaminoethyl)amino-6-(beta-diethylaminoethyl)aminonitrobenzene

시약·촉매·용매 1

HCID 962Water용매

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온도
60 °C

실험 절차

0.2 mole (45.3 g) of 2,4,6-trichloronitrobenzene is added portionwise, with stirring, to 180 ml of N,N-diethylethylenediamine, heated to 60° C. After the end of the addition, heating is continued for 30 minutes. The reaction mixture is diluted with 180 ml of iced water. The expected product precipitates. It is filtered off, washed with water and then dried under vacuum at 60° C. in the presence of phosphorus pentoxide. After recrystallization from 96° ethanol, it melts at 90° C.

후처리

  1. additionAfter the end of the addition
  2. temperatureheating
  3. customThe expected product precipitates
  4. filtrationIt is filtered off
  5. washwashed with water
  6. dry with materialdried under vacuum at 60° C. in the presence of phosphorus pentoxide
  7. customAfter recrystallization from 96° ethanol, it melts at 90° C.

출처 및 근거

ORD 기록
ord-375efb024509435290011ff3391e9493
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04992586

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