Methyl iodide → HCID 90416413, 화합물

HRID 633563노트

반응식

HRID 633563 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 90416413HCID 90416413, 화합물수율 82.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-786fd596a5ac48e49bdfde6e9a98b5d9
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321764B2

반응 노트

불러오는 중…