Hydrochloric Acid → 3-Nitrobenzohydrazide

HRID 267176

반응식

HRID 267176 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7](O)=[O:8])([O-:3])=[O:2].Cl.O.[NH2:15][NH2:16]>CO>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH:15][NH2:16])=[O:8])([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 84973-Nitrobenzoic acidHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 32914983-Nitrobenzohydrazide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 167g (1 mole) of m-nitrobenzoic acid and 160g (5 moles) of methanol was refluxed with stirring for 3 hours while a stream of dry HCl was bubbled in. A precipitate which formed on cooling to room temperature was filtered off, and dissolved in hot methanol. The solution was boiled for 10 minutes with a mixture of sodium carbonate and anhydrous calcium sulfate and was then filtered. The filtrate was stirred and refluxed while 118g (2 moles) of 85% hydrazine hydrate was added. The mixture was refluxed for 90 minutes and allowed to cool. The solid product was filtered off and recrystallized from water to give 258 g of m-nitrobenzhydrazide, m.p. 155°-155.5°C.

후처리

  1. temperaturewas refluxed
  2. customwas bubbled in
  3. customA precipitate which formed
  4. filtrationwas filtered off
  5. dissolutiondissolved in hot methanol
  6. additionThe solution was boiled for 10 minutes with a mixture of sodium carbonate and anhydrous calcium sulfate
  7. filtrationwas then filtered
  8. additionwas added
  9. temperatureThe mixture was refluxed for 90 minutes
  10. temperatureto cool
  11. filtrationThe solid product was filtered off
  12. customrecrystallized from water

출처 및 근거

ORD 기록
ord-6b28c221ca384031a8a33b4f05e7d3a8
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941749

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