1-Fluoro-2,6-dichloropyridinium Triflate → HCID 58349833, 화합물

HRID 1426663노트

반응식

HRID 1426663 반응식
[F:1][C:2]1[C:7]([C:8]2[NH:12][CH:11]=[C:10]([CH:13]=[O:14])[CH:9]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.[O-]S(C(F)(F)[F:20])(=O)=O.F[N+]1C(Cl)=CC=CC=1Cl>C(#N)C.O1CCCC1.C(=O)([O-])O.[Na+]>[F:20][C:9]1[C:10]([CH:13]=[O:14])=[CH:11][NH:12][C:8]=1[C:7]1[C:2]([F:1])=[N:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 2

HCID 27373111-Fluoro-2,6-dichloropyridinium TriflateHCID 58349828HCID 58349828, 화합물

생성물 1

HCID 58349833HCID 58349833, 화합물수율 15.2%

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매HCID 516892Sodium Bicarbonate용매

실험 절차

5-(2-Fluoropyridin-3-yl)-1H-pyrrole-3-carbaldehyde (660 mg) was dissolved in acetonitrile (30 mL) and tetrahydrofuran (30 mL), 1-fluoro-2,6-dichloropyridinium triflate (1.32 g) was added, and the mixture was stirred for 2 hr. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=3:2→3:7) to give the title compound as pale-yellow crystals (yield 110 mg, 15%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=3:2→3:7)

출처 및 근거

ORD 기록
ord-970ef6308c754e219258abd8596786ee
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933105B2

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