8-Hydroxyquinoline → Aluminium tri(quinolin-8-olate)

HRID 279398

반응식

HRID 279398 반응식
C([O-])(=O)C(C)O.[Al+3:7].C([O-])(=O)C(C)O.C([O-])(=O)C(C)O.[OH:20][C:21]1[CH:22]=[CH:23][CH:24]=[C:25]2[C:30]=1[N:29]=[CH:28][CH:27]=[CH:26]2>C(O)C>[CH:23]1[CH:22]=[C:21]([O-:20])[C:30]2[N:29]=[CH:28][CH:27]=[CH:26][C:25]=2[CH:24]=1.[CH:23]1[CH:22]=[C:21]([O-:20])[C:30]2[N:29]=[CH:28][CH:27]=[CH:26][C:25]=2[CH:24]=1.[CH:23]1[CH:22]=[C:21]([O-:20])[C:30]2[N:29]=[CH:28][CH:27]=[CH:26][C:25]=2[CH:24]=1.[Al+3:7]

참가 물질

4

반응물 2

HCID 19238-HydroxyquinolineHCID 924222-Hydroxypropanoic acid aluminium salt

생성물 1

HCID 90594Aluminium tri(quinolin-8-olate)

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Aluminum lactate, Al[CH3CH(OH)CO2]3, (10.0 g) and 8-hydroxyquinoline (16.0 g) were placed in a 250 mL round bottomed flask equipped with a magnetic stir bar and a reflux condenser. Ethanol (150 mL, denatured) was added and the cream colored slurry was stirred magnetically. The flask was heated to reflux by means of an electric heating mantle and reflux was maintained for 17 hours. Upon initial heating, the cream colored slurry gradually became yellowish in color. The yellow color intensified as the reaction progressed and the reaction mixture remained heterogeneous throughout the reflux period. After cooling, the reaction mixture was filtered and the yellow filter cake was sequentially washed with two 50 mL portions of ethanol, two 50 ml portions of distilled water, two 50 mL portions of ethanol, and two 50 mL portions of diethyl ether. The filter cake was air dried for 24 hours to give 14.9 g of tris(8-quinolinolato)aluminum as a bright yellow powder. The 1H-NMR spectrum of the powder matched that of a commercial sample of tris(8-quinolinolato)aluminum. The powder was dissolved in hot CHCl3 and filtered through a medium porosity glass frit. Addition of heptane and cooling to approximately 0° C. caused fine yellow needles of AlQ to precipitate from the yellow filtrate. the needles were collected by filtration, washed with petroleum ether, vacuum dried, and used to fabricate an electroluminescent lamp.

후처리

  1. customequipped with a magnetic stir bar and a reflux condenser
  2. temperatureThe flask was heated
  3. temperatureto reflux by means of an electric heating mantle
  4. temperaturereflux
  5. temperaturewas maintained for 17 hours
  6. temperatureUpon initial heating
  7. temperatureAfter cooling
  8. filtrationthe reaction mixture was filtered
  9. washthe yellow filter cake was sequentially washed with two 50 mL portions of ethanol, two 50 ml portions of distilled water, two 50 mL portions of ethanol, and two 50 mL portions of diethyl ether
  10. customdried for 24 hours

출처 및 근거

ORD 기록
ord-f95bc94151b3438da6a4aa4bf97ee4d4
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362339B1

연결된 노트

불러오는 중…