Iodine → HCID 178468648, 화합물

HRID 1096998노트

반응식

HRID 1096998 반응식
[I:1]I.[OH-].[K+].[NH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:12]=2)[CH:7]=[N:6]1.O.[Cl-].[NH4+]>CN(C=O)C>[I:1][C:7]1[C:8]2[C:13](=[CH:12][C:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:10][CH:9]=2)[NH:5][N:6]=1

참가 물질

6

반응물 4

HCID 807IodineHCID 14797Potassium HydroxideHCID 19737203Ethyl 1H-indazole-6-carboxylateHCID 57429219Ammonium chloride monohydrate

생성물 1

HCID 178468648HCID 178468648, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a 3.0-liter egg plant type flask, iodine (6.09 g, 24 mmol) and KOH (4.49 g, 68 mmol) were added to a DMF solution (60 mL) of ethyl 1H-indazole-6-carboxylate (4.52 g, 20 mmol), and stirred at room temperature for 2 hours. Saturated ammonium chloride water was added to it, extracted with ethyl acetate, washed with water and saturated saline water in that order, and dried with sodium sulfate. The reaction solution was filtered, concentrated, and the resulting solid was washed with a mixed solution of hexane and ethyl acetate to obtain the title compound as a yellow solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with water and saturated saline water in that order
  3. dry with materialdried with sodium sulfate
  4. filtrationThe reaction solution was filtered
  5. concentrationconcentrated
  6. washthe resulting solid was washed with a mixed solution of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-5348513a45e94c0dbbd84d72c5443c50
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138197B2

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