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Acetic Anhydride → HCID 600381, 화합물

HRID 1384839
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HRID 1384839 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=1.[CH3:11][C:12](OC(C)=O)=[O:13]>>[C:12]([C:8]1[C:4]2[CH:3]=[C:2]([CH3:1])[CH:10]=[CH:9][C:5]=2[S:6][CH:7]=1)(=[O:13])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 843465-Methylbenzo(b)thiophene

생성물 1

HCID 600381HCID 600381, 화합물수율 50%

실험 절차

1 g of 5-methylbenzo(b)thiophene (6.75×10−3 moles) was stirred at 55° C. with 0.8 ml of Ac2O (8.10×10−3 moles). 0.83 ml of BF3 Et2O were added and stirring was continued for 8 hours.11 The solvent was removed in the rotary evaporator and the residue was extracted with AcOEt and H2O. It was decanted and washed with NaHCO3 and H2O. It was dried with Na2SO4, the solvent was removed and the product was purified in successive columns of AcOEt/hexane (1:1) and toluene respectively. A product was obtained which was a mixture of the substitution isomers in positions 2- and 3- of the benzo(b)thiophene ring in a proportion of approximately 20/80 (determined by the ratios of the areas of the NMR signals), which was passed to the following reaction. Yield: 50%.

후처리

  1. custom11 The solvent was removed in the rotary evaporator
  2. extraction
the residue was extracted with AcOEt and H2O
  • customIt was decanted
  • washwashed with NaHCO3 and H2O
  • dry with materialIt was dried with Na2SO4
  • customthe solvent was removed
  • customthe product was purified in successive columns of AcOEt/hexane (1:1) and toluene respectively
  • customA product was obtained which
  • additiona mixture of the substitution isomers in positions 2-
  • customwas passed to the following reaction
  • 출처 및 근거

    ORD 기록
    ord-fc4be5a7cd23479281ebd7231ff7602b
    출처 데이터셋
    uspto-grants-2001_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06262056B1

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