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

HRID 1577050

反応式

HRID 1577050 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5190f7ef489a4519bf7ba1c9e123a25b
出典データセット
uspto-grants-1981_09
特許番号
US04286998

関連ノート

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