Hydrazine → 2-Hydrazinyl-5-iodopyridine

HRID 1372465노트

반응식

HRID 1372465 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([I:8])=[CH:4][N:3]=1.[NH2:9][NH2:10]>N1C=CC=CC=1>[I:8][C:5]1[CH:6]=[CH:7][C:2]([NH:9][NH2:10])=[N:3][CH:4]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 43971762-Chloro-5-iodopyridine

생성물 1

HCID 223971882-Hydrazinyl-5-iodopyridine

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2-chloro-5-iodopyridine (1.918 g, 8.01 mmol), anhydrous hydrazine (1.26 mL, 40.05 mmol) and pyridine (30 mL) was warmed at reflux for 18 h. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue was partitioned between dichloromethane and 1N aqueous sodium hydroxide solution. The organic layer was separated, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was triturated with hexanes, and the resultant precipitate was collected and dried in vacuo to afford the title compound as off-white crystals. LC/MS 235.8 (M+1).

후처리

  1. temperaturewas warmed
  2. temperatureat reflux for 18 h
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. customThe residue was partitioned between dichloromethane and 1N aqueous sodium hydroxide solution
  5. customThe organic layer was separated
  6. dry with materialdried (magnesium sulfate)
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was triturated with hexanes
  9. customthe resultant precipitate was collected
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-bea3ef6a301e4f3685fe133979457d6b
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157490B2

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