Dimethylformamide → Methyl 3-iodo-1-methyl-1H-indazole-6-carboxylate

HRID 1096999노트

반응식

HRID 1096999 반응식
CI.C[N:4]([CH:6]=O)[CH3:5].[I:8][C:9]1[C:17]2C(=[CH:13][C:14]([C:18]([O:20][CH2:21]C)=[O:19])=[CH:15][CH:16]=2)N[N:10]=1.C([O-])([O-])=O.[K+].[K+]>CCCCCC.C(OCC)(=O)C.CO>[I:8][C:9]1[C:17]2[C:6](=[CH:13][C:14]([C:18]([O:20][CH3:21])=[O:19])=[CH:15][CH:16]=2)[N:4]([CH3:5])[N:10]=1

참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodide2회HCID 11430Potassium Carbonate2회HCID 178468648HCID 178468648, 화합물

생성물 1

HCID 57931017Methyl 3-iodo-1-methyl-1H-indazole-6-carboxylate

시약·촉매·용매 3

HCID 887Methanol용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

In a 100-mL egg plant-type flask, MeI (381 mL, 6 mmol) was added to a DMF solution (10 ml) of ethyl 3-iodo-1H-indazole-6-carboxylate (948 mg, 3 mmol) and K2CO3 (830 mg, 6 mmol), and stirred overnight at room temperature. Further, and K2CO3 (830 mg, 6 mmol) and methyl iodide (381 μL, 6 mmol) were added to it, and stirred at 50° C. for 1 hour. After the starting materials disappeared, methanol was added to the reaction solution and stirred at that temperature for 30 minutes. This was diluted with a mixed solvent of hexane and ethyl acetate, and washed with water and saturated saline water in that order, dried with sodium sulfate, filtered, concentrated and purified through silica gel column chromatography to obtain the title compound as a colorless solid.

후처리

  1. stirringstirred at 50° C. for 1 hour
  2. stirringstirred at that temperature for 30 minutes
  3. washwashed with water and saturated saline water in that order
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified through silica gel column chromatography

출처 및 근거

ORD 기록
ord-15d2bbd61de048bca287495f53ff91dd
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138197B2

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