Methyl iodide → 2-Chloro-1-methyl-5-nitroindole-3-carbaldehyde

HRID 1957214노트

반응식

HRID 1957214 반응식
[Cl:1][C:2]1[NH:3][C:4]2[C:9]([C:10]=1[CH:11]=[O:12])=[CH:8][C:7]([N+:13]([O-:15])=[O:14])=[CH:6][CH:5]=2.[H-].[Na+].[CH3:18]I>C1COCC1>[Cl:1][C:2]1[N:3]([CH3:18])[C:4]2[C:9]([C:10]=1[CH:11]=[O:12])=[CH:8][C:7]([N+:13]([O-:15])=[O:14])=[CH:6][CH:5]=2

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 38092012-chloro-5-nitro-1H-indole-3-carbaldehyde

생성물 1

HCID 108238742-Chloro-1-methyl-5-nitroindole-3-carbaldehyde

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 5 g of (65) in 100 ml THF was added 550 mg NaH and 2.5 ml methyliodide. The reaction was left with stirring overnight. Most of the THF was evaporated off, water was added, and the water phase extracted with EtOAc. The water phase was then acidified with acetic acid, which precipitated the pure product. Filtration and drying gave 770 mg of (66).

후처리

  1. waitThe reaction was left
  2. customMost of the THF was evaporated off
  3. additionwater was added
  4. extractionthe water phase extracted with EtOAc
  5. customprecipitated the pure product
  6. filtrationFiltration
  7. customdrying

출처 및 근거

ORD 기록
ord-2ac73b4ba323450a8e575613998a422c
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05783575

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