Hydrochloric Acid → HCID 178479526, 화합물

HRID 746036노트

반응식

HRID 746036 반응식
C(=O)(O)O.[NH2:5][NH:6][C:7]([NH2:9])=[NH:8].Cl.[Cl:11][C:12]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][CH:17]=[C:16]([Cl:23])[C:13]=1[CH:14]=O>O.C(O)C>[ClH:11].[Cl:11][C:12]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][CH:17]=[C:16]([Cl:23])[C:13]=1[CH:14]=[N:5][NH:6][C:7]([NH2:9])=[NH:8]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 27949122,6-Dichloro-3-nitrobenzaldehydeHCID 178513185HCID 178513185, 화합물

생성물 1

HCID 178479526HCID 178479526, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Aminoguanidine hydrogen carbonate (1.24 g, 9.1 mmol) was added to a solution of concentrated hydrochloric acid (0.8 cm3, 9.3 mmol) in water (3 cm3). After diluting the resulting solution with ethanol (20 cm3), 2,6-dichloro-3-nitrobenzaldehyde (2.0 g, 9.1 mmol) was added and the mixture heated under reflux for 7 h. The solution was evaporated under reduced pressure and the residual solid suspended in refluxing ethanol, basified (pH 11) by addition of dilute sodium hydroxide solution and cooled to yield a white solid which was collected. This solid was dissolved in hot methanol and the solution acidified (pH 2) with ethanolic hydrogen chloride, diluted with diethyl ether and cooled to yield (2,6-dichloro-3-nitrobenzylideneamino)-guanidine hydrochloride as a white solid, m.p. 186°-7° C.

후처리

  1. additionwas added
  2. temperaturethe mixture heated
  3. temperatureunder reflux for 7 h
  4. customThe solution was evaporated under reduced pressure
  5. temperaturein refluxing ethanol
  6. additionby addition of dilute sodium hydroxide solution
  7. temperaturecooled
  8. customto yield a white solid which
  9. customwas collected
  10. dissolutionThis solid was dissolved in hot methanol
  11. additiondiluted with diethyl ether
  12. temperaturecooled

출처 및 근거

ORD 기록
ord-65cb7e0178344999b0b2991617e698d7
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04602041

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