Hydroxylamine → HCID 68138846, compound

HRID 1076664Notes

Reaction equation

HRID 1076664 reaction equation
[N+](C1O[C:7]([C:9]2[N:13]3NC(=COCC)[C:16]([NH2:18])=[CH:17][C:12]3=NN=2)=CC=1)([O-])=O.NO.Cl.NO.[Na].[N+:29]([C:32]1[O:36][C:35]([C:37]2[N:41]3[NH:42][C:43](=[CH:47][NH:48]O)[C:44]([NH2:46])=[CH:45][C:40]3=[N:39][N:38]=2)=[CH:34][CH:33]=1)([O-:31])=[O:30]>C(O)C.O1CCOCC1>[N+:29]([C:32]1[O:36][C:35]([C:37]2[N:41]3[NH:42][C:43](=[CH:47][NH:48][C:17]4[CH:16]=[N:18][C:9]([CH3:7])=[N:13][CH:12]=4)[C:44]([NH2:46])=[CH:45][C:40]3=[N:39][N:38]=2)=[CH:34][CH:33]=1)([O-:31])=[O:30]

Participants

8

Reactant 5

HCID 787HydroxylamineHCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 68140652HCID 68140652, compoundHCID 86733435HCID 86733435, compound

Product 1

HCID 68138846HCID 68138846, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 312751,4-DioxaneSolvent

Procedure

In an analogous manner, from 0.6 g. 3-(5-nitro-2-furyl)-6-(ethoxy-methylene)-amino-s-triazolo[4,3-b]pyridazine in 12 ml. anhydrous dioxan and an ethanolic solution of hydroxylamine (prepared from 0.6 g. hydroxylamine hydrochloride in 15 ml. absolute ethanol by adding 0.14 g. sodium, dissolved in 5 ml. absolute ethanol, and filtering off with suction the precipitated sodium chloride) at 50° - 60°C., there was obtained, after a reaction period of 15 minutes and cooling of the reaction mixture, 0.55 g. 3-(5-nitro-2-furyl)-6-(hydroxylaminomethylene)-amino-s-triazolo[4,3-b]pyridazine, which melted, with foaming, at 251° - 253°C.

Workup

  1. filtrationabsolute ethanol, and filtering off with suction the precipitated sodium chloride) at 50° - 60°C.
  2. customthere was obtained
  3. customafter a reaction period of 15 minutes
  4. temperaturecooling of the reaction mixture, 0.55 g
  5. custommelted, with foaming, at 251° - 253°C.

Sources & evidence

ORD record
ord-64304a03fc654fddb4b53e7c875064c7
Source dataset
uspto-grants-1976_05
Patent number
US03957766

Reaction notes

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