Hydrazine hydrate (1:1) → 2-Hydrazinyl-3-nitropyridine

HRID 963153ノート

反応式

HRID 963153 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.O.[NH2:12][NH2:13]>CO>[NH:12]([C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1)[NH2:13]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 796132-Chloro-3-nitropyridine

生成物 1

HCID 35789352-Hydrazinyl-3-nitropyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-Chloro-3-nitropyridine (100 g, 0.63 mol), hydrazine monohydrate (70.4 mL, 72.6 g, 1.45 mol) and methanol (1.3 L) were mixed and heated to reflux with stirring. After 30 min the reaction mixture was cooled and filtered collecting the insoluble materials. The filtrate was concentrated by evaporation under reduced pressure and the residue obtained as well as the insoluble materials from the filtration were diluted with water. The insoluble solids present were collected by filtration, washed with water, and dried to obtain 95.2 g (98 percent of theory) of the title compound as a bright yellow powder melting at 168°-169° C.

後処理

  1. temperatureheated
  2. temperatureto reflux
  3. temperatureAfter 30 min the reaction mixture was cooled
  4. filtrationfiltered
  5. customcollecting the insoluble materials
  6. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  7. customthe residue obtained as well as the insoluble materials
  8. filtrationfrom the filtration
  9. additionwere diluted with water
  10. filtrationThe insoluble solids present were collected by filtration
  11. washwashed with water
  12. customdried

出典と根拠

ORDレコード
ord-2009dc2bd3ad43dda02cf1ed9d7763fc
出典データセット
uspto-grants-1998_06
特許番号
US05763359

反応ノート

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