Hydrazine → 2-Hydrazinyl-5-iodopyridine

HRID 1483858ノート

反応式

HRID 1483858 の反応式
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]

参加物

4

反応物 2

HCID 9321HydrazineHCID 43971762-Chloro-5-iodopyridine

生成物 1

HCID 223971882-Hydrazinyl-5-iodopyridine収率 69%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8d7be083a5264eb78a426ca3e534fcd2
出典データセット
uspto-grants-2016_08
特許番号
US09416132B2

反応ノート

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