Iodine → HCID 178506076、化合物

HRID 246657ノート

反応式

HRID 246657 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:11]=[C:10]2[C:6]([CH:7]=[N:8][NH:9]2)=[CH:5][CH:4]=1.[OH-].[K+].[I:16]I.C(OCC)(=O)C>CN(C=O)C>[I:16][C:7]1[C:6]2[C:10](=[CH:11][C:3]([C:2]([F:1])([F:12])[F:13])=[CH:4][CH:5]=2)[NH:9][N:8]=1

参加物

6

反応物 4

HCID 807IodineHCID 8857Ethyl AcetateHCID 14797Potassium HydroxideHCID 214555996-(trifluoromethyl)-1H-indazole

生成物 1

HCID 178506076HCID 178506076、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6-(trifluoromethyl)-1H-indazole (0.5 g, 2.69 mmol), KOH (0.45 g, 8.1 mmol) and I2 (1.37 g, 5.38 mmol) in dry DMF (20 mL) was stirred for 16 hours at room temperature. Ethyl acetate (100 mL) was added and the mixture was washed with water (3×10 mL) and brine (2×10 mL). The organic layer was dried over Na2SO4, filtered and concentrated. The residue was then washed with ether (2 mL) and filtered to afford 3-iodo-6-(trifluoromethyl)-1H-indazole (688 mg, crude) as a yellow solid. LCMS: (M+H)+=313.

後処理

  1. washthe mixture was washed with water (3×10 mL) and brine (2×10 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washThe residue was then washed with ether (2 mL)
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-cd327757b8ee494fabab218089ea018b
出典データセット
uspto-grants-2014_02
特許番号
US08658646B2

反応ノート

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