Iodine → HCID 178468648、化合物

HRID 1096998ノート

反応式

HRID 1096998 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 178468648HCID 178468648、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5348513a45e94c0dbbd84d72c5443c50
出典データセット
uspto-grants-2012_03
特許番号
US08138197B2

反応ノート

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