Methyl iodide → HCID 90416413、化合物

HRID 633563ノート

反応式

HRID 633563 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[CH:11]=[CH:10][NH:9][C:5]2=[C:6]([Cl:8])[N:7]=1.[H-].[Na+].I[CH3:15]>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]2[CH:11]=[CH:10][N:9]([CH3:15])[C:5]2=[C:6]([Cl:8])[N:7]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 467379065-Bromo-7-chloro-1H-pyrrolo[2,3-c]pyridine

生成物 1

HCID 90416413HCID 90416413、化合物収率 82.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 5-bromo-7-chloro-1H-pyrrolo[2,3-c]pyridine (Aldrich, 0.86 g, 3.72 mmol) in tetrahydrofuran (37.2 mL) was treated with sodium hydride (0.297 g, 7.43 mmol) at ambient temperature, stirred for 15 minutes, treated with iodomethane (0.348 mL, 5.57 mmol), stirred for 1 hour at ambient temperature and quenched with saturated aqueous ammonium chloride. The mixture was partitioned with ethyl acetate and the organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), filtered, and concentrated. Purification by chromatography (silica gel, 0-40% ethyl acetate in heptanes) afforded the title compound (0.75 g, 82%).

後処理

  1. stirringstirred for 1 hour at ambient temperature
  2. customquenched with saturated aqueous ammonium chloride
  3. customThe mixture was partitioned with ethyl acetate
  4. washthe organic layer was washed with saturated aqueous sodium chloride
  5. dry with materialdried (anhydrous Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customPurification by chromatography (silica gel, 0-40% ethyl acetate in heptanes)

出典と根拠

ORDレコード
ord-786fd596a5ac48e49bdfde6e9a98b5d9
出典データセット
uspto-grants-2016_04
特許番号
US09321764B2

反応ノート

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