1-Chloroanthraquinone → 1-(1-Ethylpropylamino)anthraquinone

HRID 1376307

반응식

HRID 1376307 반응식
Cl[C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH2:18]([CH:20]([NH2:23])[CH2:21][CH3:22])[CH3:19].C([O-])(=O)C.[K+]>[Cu].O>[CH2:18]([CH:20]([NH:23][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1)[CH2:21][CH3:22])[CH3:19]

참가 물질

6

반응물 3

HCID 67091-ChloroanthraquinoneHCID 120193-PentanamineHCID 517044Potassium Acetate

생성물 1

HCID 229162751-(1-Ethylpropylamino)anthraquinone

시약·촉매·용매 2

HCID 23978Copper촉매HCID 962Water용매

반응 조건

온도
180 °C

실험 절차

A Parr stainless steel high pressure reactor was charged with 1-chloroanthraquinone (24.3 g), 1-ethylpropylamine (17.5 g), potassium acetate.(14.0 g), activated copper metal (0.7 g), and water (0.05 g). The reaction vessel was sealed and heated to a temperature of 180° C. in an oil bath and maintained at that temperature for 12 hours. The oil bath was removed and the vessel was allowed to return to ambient conditions. The solid was extracted with methylene chloride and the insoluble materials removed by filtration. The solvent was removed and the solid recrystallized from hot methanol. The material was chromatographed on a silica gel column using toluene as the eluent.

후처리

  1. customThe reaction vessel was sealed
  2. temperaturemaintained at that temperature for 12 hours
  3. customThe oil bath was removed
  4. extractionThe solid was extracted with methylene chloride
  5. customthe insoluble materials removed by filtration
  6. customThe solvent was removed
  7. customthe solid recrystallized from hot methanol
  8. customThe material was chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-4b619910aa744d42828a8ffc7b87d55a
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663024

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