N-Iodosuccinimide → HCID 178505409、化合物

HRID 34129ノート

反応式

HRID 34129 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 178505409HCID 178505409、化合物収率 91.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-a8cb828c57634091a7280e761e4badb3
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

反応ノート

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