Iodine → HCID 178506076, 화합물

HRID 246657노트

반응식

HRID 246657 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 178506076HCID 178506076, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cd327757b8ee494fabab218089ea018b
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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