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Dimethylformamide → 3-Chloro-4-(2-chloro-3,6-dimethyl-4-nitrophenoxy)-1,1'-biphenyl

HRID 980565
ノート
印刷プレビュー

反応式

HRID 980565 の反応式
[CH3:1][C:2]1[C:7]([Cl:8])=[C:6](Cl)[C:5]([CH3:10])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[Cl:14][C:15]1[CH:20]=[C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:18]=[CH:17][C:16]=1[OH:27].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>C1(C)C=CC=CC=1>[Cl:14][C:15]1[CH:20]=[C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:18]=[CH:17][C:16]=1[O:27][C:6]1[C:5]([CH3:10])=[CH:4][C:3]([N+:11]([O-:13])=[O:12])=[C:2]([CH3:1])[C:7]=1[Cl:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 70742-Chloro-4-PhenylphenolHCID 11430Potassium CarbonateHCID 137729272,3-Dichloro-1,4-dimethyl-5-nitrobenzene

生成物 1

HCID 137729283-Chloro-4-(2-chloro-3,6-dimethyl-4-nitrophenoxy)-1,1'-biphenyl収率 71.6%

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

実験手順

Into a 100 milliliter round bottom flask equipped with a thermometer, magnetic stirrer and condenser was added 12.0 grams (0.054 moles) of 2,5-dimethyl-3,4-dichloronitrobenzene, 14.5 grams (0.071 moles) of 2-chloro-4-phenylphenol, 12.0 grams (0.087 moles) of potassium carbonate and 20 milliliters of dimethylformamide (DMF) under a nitrogen atmosphere at ambient temperature. The reaction mixture was then heated in an oil bath at a temperature of 110° C.-120° C. for a periof of 72 hours. After cooling to ambient temperature, the reaction mixture was filtered through celite and concentrated (DMF removed under vaccum) to give an amber oil. The amber oil was dissolved in toluene and thereafter washed once with 4% sodium hydroxide, once with water and finally once with a saturated aqueous sodium chloride solution. The amber oil was then dried over sodium sulfate, concentrated (toluene removed under vacuum) and stirred into a hexane-ethyl acetate mixture (6:1 volume ratio). Crystallization from the hexane-ethyl acetate mixture and filtration afforded 15.02 grams of a tan powder having a melting point of 92.5° C.-94.0° C. Elemental analysis of the tan powder indicated the following:

後処理

  1. customInto a 100 milliliter round bottom flask equipped with a thermometer, magnetic stirrer and condenser
  2. temperatureThe reaction mixture was then heated in an oil bath at a temperature of 110° C.-120° C. for a periof of 72 hours
  3. filtrationthe reaction mixture was filtered through celite and
  4. concentrationconcentrated
  5. custom(DMF removed under vaccum)
  6. customto give an amber oil
  7. washwashed once with 4% sodium hydroxide, once with water and finally once with a saturated aqueous sodium chloride solution
  8. dry with materialThe amber oil was then dried over sodium sulfate
  9. concentrationconcentrated
  10. custom(toluene removed under vacuum)
  11. customCrystallization
  12. filtrationfrom the hexane-ethyl acetate mixture and filtration

出典と根拠

ORDレコード
ord-6779a32fd76b4b16a1e8438d02af82fc
出典データセット
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04638088

反応ノート

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