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

HRID 1735110노트

반응식

HRID 1735110 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-31f63e112e3f425db993048849140007
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05536721

반응 노트

불러오는 중…