Benzene → HCID 15434853、化合物

HRID 1604454ノート

反応式

HRID 1604454 の反応式
[Br:1][C:2]1[O:3][C:4](Br)=[CH:5][CH:6]=1.[CH:8]1C=C[CH:11]=[CH:10][CH:9]=1.C([O-])([O-])=[O:15].[Na+].[Na+]>CO.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Br:1][C:2]1[O:3][C:4]([C:8]2[O:15][CH:11]=[CH:10][CH:9]=2)=[CH:5][CH:6]=1

参加物

6

反応物 3

HCID 241BenzeneHCID 10340Sodium CarbonateHCID 108788462,5-dibromofuran

生成物 1

HCID 15434853HCID 15434853、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 887Methanol溶媒

実験手順

In a 2-neck flask was placed 2,5-dibromofuran (18.1 g, 80 mmol) with catalyst Pd(PPh3)4 (5 mol %) and added 30 mL of benzene and 6 mL of 2 M Na2CO3 aqueous solution. The mixture was added 2.2 g (20 mmol) of dihydroxy-2-(furyl) borane dissolved in 6 mL of methanol and heated at reflux for 12 hrs. Thin layer chromatography ("TLC") showed 2 fluorescent spots. The less polar spot was identified as the desired dimer product. The mixture was extracted with ether. The combined ether extracts were dried with anhydrous MgSO4 and concentrated. The crude product was then used for the next reaction.

後処理

  1. customIn a 2-neck flask was placed
  2. temperatureheated
  3. temperatureat reflux for 12 hrs
  4. extractionThe mixture was extracted with ether
  5. dry with materialThe combined ether extracts were dried with anhydrous MgSO4
  6. concentrationconcentrated
  7. customThe crude product was then used for the next reaction

出典と根拠

ORDレコード
ord-1f29d136d5734e09a5e4a56c194d17f2
出典データセット
uspto-grants-1999_11
特許番号
US05994394

反応ノート

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