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

HRID 1735110ノート

反応式

HRID 1735110 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-31f63e112e3f425db993048849140007
出典データセット
uspto-grants-1996_07
特許番号
US05536721

反応ノート

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