Benzene → HCID 15434853, 화합물

HRID 1604454노트

반응식

HRID 1604454 반응식
[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

참가 물질

6

반응물 3

HCID 241BenzeneHCID 10340Sodium CarbonateHCID 108788462,5-dibromofuran

생성물 1

HCID 15434853HCID 15434853, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1f29d136d5734e09a5e4a56c194d17f2
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05994394

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