Iodine → HCID 178455023, 화합물

HRID 245951

반응식

HRID 245951 반응식
[C:1]([Si:5]([CH3:17])([CH3:16])[O:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][N:11]=[CH:10]2)([CH3:4])([CH3:3])[CH3:2].[I:18]I.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:1]([Si:5]([CH3:17])([CH3:16])[O:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][N:11]=[C:10]2[I:18])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 807IodineHCID 11430Potassium CarbonateHCID 580425115-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]-1H-indazole

생성물 1

HCID 178455023HCID 178455023, 화합물수율 91.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a round-bottomed flask, 5-(tert-butyl-dimethyl-silanyloxy)-1H-indazole (1.20 g, 4.83 mmol) was dissolved in DMF (12 ml). Iodine (2.45 g, 9.66 mmol) was added followed by potassium carbonate (2.58 g, 18.7 mmol). The dark suspension was stirred at room temperature for 3 h then quenched with 10% aqueous NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed with 10% aqueous NaHSO3, three times with water and once with brine then dried over sodium sulfate, filtered and concentrated to afford 1.65 g (91%) of 5-(tert-butyl-dimethyl-silanyloxy)-3-iodo-1H-indazole as a dark brown foam.

후처리

  1. customthen quenched with 10% aqueous NaHSO3
  2. extractionextracted with diethyl ether (2×)
  3. washThe combined organic layers were washed with 10% aqueous NaHSO3, three times with water and once with brine
  4. dry with materialthen dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ab11783009c84a739eb510414586ec03
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

연결된 노트

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