Potassium Carbonate → HCID 19708511、化合物

HRID 725746ノート

反応式

HRID 725746 の反応式
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:14][C:15]1[CH:16]=[C:17]([C:22]2[CH:27]=[CH:26][C:25](I)=[C:24]([CH3:29])[CH:23]=2)[CH:18]=[CH:19][C:20]=1[I:21].C(=O)([O-])[O-].[K+].[K+]>[Cu].[N+](C1C=CC=CC=1)([O-])=O>[CH3:29][C:24]1[CH:23]=[C:22]([C:17]2[CH:18]=[CH:19][C:20]([I:21])=[C:15]([CH3:14])[CH:16]=2)[CH:27]=[CH:26][C:25]=1[N:7]([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 11487DiphenylamineHCID 223236094,4'-Diiodo-3,3'-dimethyl-1,1'-biphenyl

生成物 1

HCID 19708511HCID 19708511、化合物収率 57.2%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 7416Nitrobenzene溶媒

実験手順

20.3 g (0.12 mol) of diphenylamine, 65.1 g (0.15 mol) of 3,3'-dimethyl-4,4'-diiodobiphenyl, 19.3 g (0.14 mol) of anhydrous potassium carbonate, 1.52 g (0.024 mol) of copper powder, and 20 ml of nitrobenzene were mixed. The reaction mixture was then allowed to undergo reaction at a temperature of 190° C. to 205° C. for 21 hours. The reaction product was then extracted with 200 ml of toluene. The insoluble contents were removed by filtration. The filtrate was then concentrated to dryness. The concentrate was then purified by column chromatography (carrier: silica gel; elute: 2/7 mixture of toluene and n-hexane) to obtain 32.6 g (yield: 57.2%) of N-(3,3'-dimethyl-4'-iodo-4-biphenylyl)-N,N-diphenylamine.

後処理

  1. customreaction at a temperature of 190° C. to 205° C. for 21 hours
  2. extractionThe reaction product was then extracted with 200 ml of toluene
  3. customThe insoluble contents were removed by filtration
  4. concentrationThe filtrate was then concentrated to dryness
  5. customThe concentrate was then purified by column chromatography (carrier: silica gel; elute: 2/7 mixture of toluene and n-hexane)

出典と根拠

ORDレコード
ord-c7517e6b1b434c73acc77f86d5acd191
出典データセット
uspto-grants-1998_01
特許番号
US05707747

反応ノート

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