Methyl iodide → 1H-Indole, 2,3-dihydro-1-methyl-5-nitro-

HRID 450040

반응식

HRID 450040 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][CH2:8][CH2:7]2)([O-:3])=[O:2].[OH-].[K+].[CH3:15]I>CC(C)=O>[CH3:15][N:9]1[C:10]2[C:6](=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=2)[CH2:7][CH2:8]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 362195-Nitroindoline

생성물 1

HCID 1677381H-Indole, 2,3-dihydro-1-methyl-5-nitro-수율 92%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 5-nitroindoline (1.0 g, 6.1 mmol) in acetone (12 ml), powdered potassium hydroxide (1.7 g, 30.5 mmol, 5 eq) was added followed by the addition of methyl iodide (1.2 g, 9.1 mmol, 1.5 eq) at 0° C. The reaction mixture was stirred at room temperature overnight. The solvent was evaporated and water was added and the compound was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated to dryness to yield 1-methyl-5-nitro-2,3-dihydro-1H-indole (1.0 g, 92%). The crude compound was used in the next stage without purification.

후처리

  1. customThe solvent was evaporated
  2. additionwater was added
  3. extractionthe compound was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-dbef5ae2e9084970b97682d86da42dcd
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486962B2

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