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

HRID 441106

반응식

HRID 441106 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-4695c54ee1f1423bbc8ddde782de8afb
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521271

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