O-Phenylenediamine → 2,3-Bis(p-hydroxyphenyl)quinoxaline

HRID 1085643

반응식

HRID 1085643 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH2:8].[OH:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:18]([C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=2)=O)=O)=[CH:12][CH:11]=1>C(O)C>[OH:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2[C:18]([C:20]3[CH:21]=[CH:22][C:23]([OH:26])=[CH:24][CH:25]=3)=[N:8][C:3]3[C:2](=[CH:7][CH:6]=[CH:5][CH:4]=3)[N:1]=2)=[CH:14][CH:15]=1

참가 물질

4

반응물 2

HCID 7243O-PhenylenediamineHCID 4582044,4'-Dihydroxybenzil

생성물 1

HCID 4591402,3-Bis(p-hydroxyphenyl)quinoxaline수율 97.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Into a 250 ml round bottom flask equipped with a magnetic stirrer and reflux condenser was placed 1,2-diaminobenzene (2.3275 g, 0.0215 mol), 4,4'-dihydroxybenzil (5.2135 g, 0.0215 mol) and absolute ethanol (30 ml). The solution was stirred for one-half hour at room temperature, and a yellow precipitate formed. The mixture was heated to reflux overnight. The solvent was removed by vacuum distillation and the solid dried at 100° C. for two hours to give 6.6 g (97%) of yellow powder. The material was recrystallized from 1,4-dioxane/water mixture. Yield 6.0 g (89%) m.p. 336° C.-338° C. Anal. Calcd for C20H14N2O2 : C, 76.42%; H, 4.49%; N, 8.91%. Found: C, 76.54%; H, 4.44%; N,8.96%.

후처리

  1. customInto a 250 ml round bottom flask equipped with a magnetic stirrer
  2. temperaturereflux condenser
  3. customa yellow precipitate formed
  4. temperatureThe mixture was heated
  5. temperatureto reflux overnight
  6. customThe solvent was removed by vacuum distillation
  7. customthe solid dried at 100° C. for two hours

출처 및 근거

ORD 기록
ord-62ac2e4558394bfea352a345c14fb9a5
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05010197

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