Iodine → HCID 178468692, 화합물

HRID 34045노트

반응식

HRID 34045 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7]([O:15][CH3:16])=[C:8]2[C:12](=[CH:13][CH:14]=1)[NH:11][N:10]=[CH:9]2)=[O:5])[CH3:2].[I:17]I.[OH-].[K+].S([O-])(O)=O.[Na+]>CN(C)C=O>[CH2:1]([O:3][C:4]([C:6]1[C:7]([O:15][CH3:16])=[C:8]2[C:12](=[CH:13][CH:14]=1)[NH:11][N:10]=[C:9]2[I:17])=[O:5])[CH3:2]

참가 물질

6

반응물 4

HCID 807Iodine2회HCID 14797Potassium HydroxideHCID 23665763Sodium BisulfiteHCID 59797354CID 59797354

생성물 1

HCID 178468692HCID 178468692, 화합물수율 80.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 15 mL of a solution of 1.33 g of 4-methoxy-1H-indazole-5-carboxylic acid ethyl ester in N,N-dimethylformamide were added 1.95 g of iodine and 0.85 g of potassium hydroxide, stirred at room temperature for 1 hour and 40 minutes, added with another 0.8 g of iodine, and stirred for 3 hours and 20 minutes. Thereafter, 10% sodium hydrogen sulfite aqueous solution was added, extracted twice with ethyl acetate, and the organic layer was washed once with saturated brine, dried over magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography, to afford 1.68 g of the title compound as colorless crystals.

후처리

  1. stirringstirred for 3 hours and 20 minutes
  2. extractionextracted twice with ethyl acetate
  3. washthe organic layer was washed once with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated
  6. customThe crude product was purified
  7. customseparated by silica gel column chromatography

출처 및 근거

ORD 기록
ord-76b38609be7a41c29b6c85e3479acf20
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429609B2

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