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

HRID 1957214ノート

反応式

HRID 1957214 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2ac73b4ba323450a8e575613998a422c
出典データセット
uspto-grants-1998_07
特許番号
US05783575

反応ノート

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