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

HRID 260817

반응식

HRID 260817 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 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. customThe oil bath was removed
  3. extractionThe solid was extracted with methylene chloride
  4. customthe insoluble materials removed by filtration
  5. customThe solvent was removed
  6. customthe solid recrystallized from hot methanol
  7. customThe material was chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-900e32d5cc3c440e9f39f7144b589599
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530067

연결된 노트

불러오는 중…