N-Iodosuccinimide → HCID 178505409, 화합물

HRID 34129

반응식

HRID 34129 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][N:6]=[CH:5]2.[I:12]N1C(=O)CCC1=O>CN(C)C=O.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][N:6]=[C:5]2[I:12]

참가 물질

5

반응물 2

HCID 120273N-IodosuccinimideHCID 468639235-Bromo-6-fluoro-1H-indazole

생성물 1

HCID 178505409HCID 178505409, 화합물수율 91.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
70 °C

실험 절차

To a solution of 10.0 g of 5-bromo-6-fluoro-1H-indazole in 150 mL of N,N-dimethylformamide was added 10.5 g of N-iodosuccinimide at room temperature, and stirred at 70° C. for 2 days. Then the solution was diluted with ethyl acetate, washed successively with aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crystals precipitated by adding diethyl ether to the residue were collected by filtration. The filtrate was further concentrated and purified and separated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5) and combined with the previous crystals, to afford 14.5 g of the title compound as colorless crystals.

후처리

  1. washwashed successively with aqueous ammonium chloride and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated
  4. customThe crystals precipitated
  5. additionby adding diethyl ether to the residue
  6. filtrationwere collected by filtration
  7. concentrationThe filtrate was further concentrated
  8. custompurified
  9. customseparated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5)

출처 및 근거

ORD 기록
ord-a8cb828c57634091a7280e761e4badb3
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429609B2

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