Hydrochloric Acid → HCID 178479526、化合物

HRID 746036ノート

反応式

HRID 746036 の反応式
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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 27949122,6-Dichloro-3-nitrobenzaldehydeHCID 178513185HCID 178513185、化合物

生成物 1

HCID 178479526HCID 178479526、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-65cb7e0178344999b0b2991617e698d7
出典データセット
uspto-grants-1986_07
特許番号
US04602041

反応ノート

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