1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → 9(10H)-Acridinone, 2-(phenylamino)-

HRID 1577050

반응식

HRID 1577050 반응식
[NH:1]([C:8]1[CH:21]=[CH:20][C:19]2[NH:18][C:17]3[CH2:16][CH2:15][CH2:14][CH2:13][C:12]=3[C:11](=[O:22])[C:10]=2[CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[Pd]>[NH:1]([C:8]1[CH:21]=[CH:20][C:19]2[NH:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:22])[C:10]=2[CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 140291045,6,7,8-Tetrahydro-2-anilinoacridone

생성물 1

HCID 30185969(10H)-Acridinone, 2-(phenylamino)-수율 89%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

A mixture of 70 g of 5,6,7,8-tetrahydro-2-anilinoacridone and 700 ml of Dowtherm® A was brought to reflux in a 2-liter resin kettle, in a nitrogen atmosphere. A stainless steel mesh basket containing 14.5 g of 0.5% palladium on 1/8 inch alumina pellets was lowered into the reaction mixture. The mixture was refluxed for 18 hours. The basket was removed from the reaction mixture, which was then allowed to cool. The precipitated product was collected on a filter and washed with four 350 ml aliquots of methanol. Vacuum oven drying at 100° C. overnight gave 61.4 g (89%) of the product that was analyzed by microanalysis.

후처리

  1. temperatureThe mixture was refluxed for 18 hours
  2. customThe basket was removed from the reaction mixture, which
  3. temperatureto cool
  4. customThe precipitated product was collected on
  5. filtrationa filter
  6. washwashed with four 350 ml aliquots of methanol
  7. customVacuum oven drying at 100° C. overnight

출처 및 근거

ORD 기록
ord-5190f7ef489a4519bf7ba1c9e123a25b
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04286998

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