Hydrazine hydrate (1:1) → HCID 434319, compound

HRID 1413931Notes

Reaction equation

HRID 1413931 reaction equation
[OH:1][CH2:2][CH2:3][N:4]([CH2:22][CH2:23][OH:24])[C:5]1[N:6]=[N:7][C:8]([N:11]2[C:15]([NH2:16])=[C:14]([C:17]([O:19]CC)=O)[CH:13]=[N:12]2)=[CH:9][CH:10]=1.O.[NH2:26][NH2:27]>O1CCOCC1>[OH:24][CH2:23][CH2:22][N:4]([CH2:3][CH2:2][OH:1])[C:5]1[N:6]=[N:7][C:8]([N:11]2[C:15]([NH2:16])=[C:14]([C:17](=[O:19])[NH:26][NH2:27])[CH:13]=[N:12]2)=[CH:9][CH:10]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 12562798HCID 12562798, compound

Product 1

HCID 434319HCID 434319, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A mixture of 6.72 g. (20 mmoles) of 3-[bis(hydroxyethyl)-amino]-6-(4-ethoxycarbonyl-5-amino-1-pyrazolyl)-pyridazine (prepared according to Example 2), 34 ml. of 72% hydrazine hydrate and 34 ml. of dioxane is stirred at reflux temperature for 12 hours. After cooling the separated crystals are filtered, washed with water and ethanol and then recrystallized from 30 ml. of ethanol. Yield: 5.7 g. (88.5%); m.p.: 217°-219° C.

Workup

  1. additionA mixture of 6.72 g
  2. temperatureat reflux temperature for 12 hours
  3. temperatureAfter cooling the separated crystals
  4. filtrationare filtered
  5. washwashed with water and ethanol
  6. customrecrystallized from 30 ml

Sources & evidence

ORD record
ord-e2e30b872c1346b594290a21bf508bf2
Source dataset
uspto-grants-1981_02
Patent number
US04251658

Reaction notes

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