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

HRID 963153노트

반응식

HRID 963153 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 35789352-Hydrazinyl-3-nitropyridine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2009dc2bd3ad43dda02cf1ed9d7763fc
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763359

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