Sodium ethoxide → HCID 58136909, compound

HRID 217682Notes

Reaction equation

HRID 217682 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-48a7a6cdd9cf417d8a062e1e7985c7cf
Source dataset
uspto-grants-2012_06
Patent number
US08198272B2

Reaction notes

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