Iodine → HCID 178505824、化合物

HRID 246096ノート

反応式

HRID 246096 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][NH:8]2)=[C:4]([F:11])[CH:3]=1.[I:12]I.[OH-].[K+].S([O-])([O-])(=O)=S.[Na+].[Na+]>CN(C=O)C.C(OCC)C.O>[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([I:12])=[N:7][NH:8]2)=[C:4]([F:11])[CH:3]=1

参加物

8

反応物 4

HCID 807IodineHCID 14797Potassium HydroxideHCID 24477Sodium ThiosulfateHCID 247284446-Chloro-4-fluoro-1H-indazole

生成物 1

HCID 178505824HCID 178505824、化合物収率 85%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

6-Chloro-4-fluoro-1H-indazole (7.6 g, 44.6 mmol) was dissolved in DMF (110 ml). Iodine (22.6 g, 89.1 mmol) was added followed by potassium hydroxide (9.5 g, 169 mmol). The reaction was stirred at room temperature for 1.5 h. Water, 1 M sodium thiosulfate solution and diethyl ether were added. The layers were separated and the aqueous layer was extracted once more with ether. The organic layers were washed with water and sodium chloride solution, and then dried over sodium sulfate. Evaporation of the solvent gave 11.16 g (85%) of 6-chloro-4-fluoro-3-iodo-1H-indazole as a light brown solid (M−H)−=295.

後処理

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted once more with ether
  3. washThe organic layers were washed with water and sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-a2a8828b2d854260a74ffecd18914479
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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