Hydrazine hydrate (1:1) → 2-Hydrazinyl-3-iodo-4-methylpyridine

HRID 2096986ノート

反応式

HRID 2096986 の反応式
Cl[C:2]1[C:7]([I:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1.O.[NH2:11][NH2:12]>N1C=CC=CC=1>[NH:11]([C:2]1[C:7]([I:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1)[NH2:12]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 451082072-Chloro-3-iodo-4-methylpyridine

生成物 1

HCID 581543012-Hydrazinyl-3-iodo-4-methylpyridine収率 87%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 2-chloro-3-iodo-4-methylpyridine (preparation 28a, 2.0 g, 7.9 mmol) and hydrazine hydrate (1.2 mL, 24.2 mmol) in pyridine (12 mL) under an argon atmosphere was stirred and heated to reflux. After 24 hours, the mixture was cooled and evaporated to dryness. The crude mixture was triturated with water and the solid was filtered and washed with water to give the title compound (1.71 g, 87%) which was used without further purification in the next reaction.

後処理

  1. temperatureheated to reflux
  2. temperaturethe mixture was cooled
  3. customevaporated to dryness
  4. customThe crude mixture was triturated with water
  5. filtrationthe solid was filtered
  6. washwashed with water

出典と根拠

ORDレコード
ord-a29fe50d7b4c424f8c8843fbd62557c8
出典データセット
uspto-grants-2013_05
特許番号
US08450341B2

反応ノート

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