Iodine → HCID 178455023、化合物

HRID 246718

反応式

HRID 246718 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 178455023HCID 178455023、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-141fc4217c0e4b0dbff96dcea8947c54
出典データセット
uspto-grants-2014_02
特許番号
US08658646B2

関連ノート

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