Sodium ethoxide → HCID 58136909, compound

HRID 657888Notes

Reaction equation

HRID 657888 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

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-c17ed502f2a0406294aafe8311bd0ec5
Source dataset
uspto-grants-2011_12
Patent number
US08076336B2

Reaction notes

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