Hydrazine → 2-Hydrazinyl-5-iodopyridine

HRID 1483858노트

반응식

HRID 1483858 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>[NH:9]([C:2]1[CH:7]=[CH:6][C:5]([I:8])=[CH:4][N:3]=1)[NH2:10]

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 43971762-Chloro-5-iodopyridine

생성물 1

HCID 223971882-Hydrazinyl-5-iodopyridine수율 69%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

The solution of 2-chloro-5-iodopyridine (2.0 g, 20.9 mmol), anhydrous hydrazine (3.3 mL, 105 mmol) in pyridine (40 mL) was heated at reflux overnight. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. To the residue was added 1 N sodium hydroxide solution and it was extracted with EtOAc. The organic layer was separated, dried (sodium sulfate) and concentrated under reduced pressure. To the residue was added hexanes, and the precipitate was collected and dried in vacuo to afford the title compound (1.35 g, 69% yield) as off-white crystals. MS (ES+, m/z): 236.2 (M++1).

후처리

  1. temperatureat reflux overnight
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added 1 N sodium hydroxide solution and it
  4. extractionwas extracted with EtOAc
  5. customThe organic layer was separated
  6. dry with materialdried (sodium sulfate)
  7. concentrationconcentrated under reduced pressure
  8. additionTo the residue was added hexanes
  9. customthe precipitate was collected
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-8d7be083a5264eb78a426ca3e534fcd2
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09416132B2

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