Hydrazine hydrate (1:1) → 2-Hydrazinyl-5-Methylpyridine

HRID 242249

反応式

HRID 242249 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1.O.[NH2:10][NH2:11]>C(OCCO)C>[NH:10]([C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1)[NH2:11]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 5813932-Chloro-5-methyl-pyridine

生成物 1

HCID 41533962-Hydrazinyl-5-Methylpyridine

試薬・触媒・溶媒 1

HCID 8076Glycol monoethyl ether溶媒

実験手順

1.0 g (7.8 mmol) 2-chloro-5-methylpyridine are stirred under reflux in 5.7 ml (5.9 g, 117.6 mmol) hydrazine hydrate for 12 h. 10 ml ethylene glycol monoethyl ether are added to the cooled reaction mixture and the solvent is then removed completely on a rotary evaporator. This working step is repeated twice, methylene chloride is then added to the residue, the precipitate is filtered off, the filtrate is concentrated in vacuo and the residue is dried in vacuo.

後処理

  1. customthe solvent is then removed completely on a rotary evaporator
  2. additionmethylene chloride is then added to the residue
  3. filtrationthe precipitate is filtered off
  4. concentrationthe filtrate is concentrated in vacuo
  5. customthe residue is dried in vacuo

出典と根拠

ORDレコード
ord-09437959471c43c8a62ecda9e00c3d66
出典データセット
uspto-grants-2014_02
特許番号
US08653111B2

関連ノート

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