Sodium ethoxide → HCID 58136909, compound

HRID 532332Notes

Reaction equation

HRID 532332 reaction equation
Cl[C:2]1[C:3]([N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])=[CH:4][C:5]2[N:6]([C:8]([NH2:11])=[N:9][N:10]=2)[N:7]=1.[O-:17][CH2:18][CH3:19].[Na+]>C(O)C>[CH2:18]([O:17][C:2]1[C:3]([N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])=[CH:4][C:5]2[N:6]([C:8]([NH2:11])=[N:9][N:10]=2)[N:7]=1)[CH3:19]

Participants

4

Reactant 2

HCID 2723922Sodium ethoxideHCID 58136956HCID 58136956, compound

Product 1

HCID 58136909HCID 58136909, compoundYield 75.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

6-Chloro-N*7*,N*7*-diethyl-[1,2,4]triazolo[4,3-b]pyridazine-3,7-diamine (W2.021, 38 mg) were initially charged in ethanol (7 ml) and admixed with sodium ethoxide (24 mg). The reaction mixture stirred at RT for 4 h. It was then stirred at 45° C. for another 2 h. Subsequently, the mixture was dried, the residue was admixed with water and extracted three times with EA, and the combined EA phases were dried with magnesium sulfate, filtered and concentrated. 30 mg of the title compound were obtained as a crude product, which was clean enough for the next reaction.

Workup

  1. stirringIt was then stirred at 45° C. for another 2 h
  2. customSubsequently, the mixture was dried
  3. extractionextracted three times with EA
  4. dry with materialthe combined EA phases were dried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-d58f273a70ad479ca2edb1a29f2735fe
Source dataset
uspto-grants-2014_10
Patent number
US08853206B2

Reaction notes

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