Iodine → HCID 178505824, 화합물

HRID 246096노트

반응식

HRID 246096 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 178505824HCID 178505824, 화합물수율 85%

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a2a8828b2d854260a74ffecd18914479
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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