Iodine → HCID 178455023, 화합물

HRID 246718

반응식

HRID 246718 반응식
[Si:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][N:13]=[CH:12]2)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH-].[K+].[I:20]I>CS(C)=O>[Si:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][N:13]=[C:12]2[I:20])([C:4]([CH3:7])([CH3:5])[CH3:6])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 807IodineHCID 14797Potassium HydroxideHCID 580425115-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]-1H-indazole

생성물 1

HCID 178455023HCID 178455023, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a stirred solution of 5-(tert-butyldimethylsilyloxy)-1H-indazole (5.3 g, 0.02 mol) in DMSO (50 mL) at 0° C., was added KOH (3.36 g, 0.06 mol) followed by iodine (10.2 g, 0.04 mol) portionwise. The mixture was stirred at room temperature for additional 10 minutes, then the reaction was quenched with 10% Na2S2O3 and diluted with water. The mixture was filtered and the filter cake was washed with water and dried to give 5-(tert-butyldimethylsilyloxy)-3-iodo-1H-indazole. The crude solid was used in the next step without purification. MS: (M+H)+=375.

후처리

  1. customthe reaction was quenched with 10% Na2S2O3
  2. additiondiluted with water
  3. filtrationThe mixture was filtered
  4. washthe filter cake was washed with water
  5. customdried

출처 및 근거

ORD 기록
ord-141fc4217c0e4b0dbff96dcea8947c54
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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